3-Chloro-2-fluorobenzaldehyde synthesis
- Product Name:3-Chloro-2-fluorobenzaldehyde
- CAS Number:85070-48-0
- Molecular formula:C7H4ClFO
- Molecular Weight:158.56
261723-30-2
85070-48-0
36.3 g of sodium bicarbonate and 500 g of dichloromethane were added to a 1 L four-necked flask, followed by 0.5 g of TOMO as a catalyst. The reaction mixture was cooled to 0 to 5°C with stirring. To this cooled mixture was slowly added a mixed solution of 50 g of (3-chloro-2-fluorophenyl)methanol and 100 g of dichloromethane. Next, 230 g of sodium hypochlorite solution was added slowly and dropwise. The reaction mixture was held at 0 to 5°C for 1 hour. The progress of the reaction was monitored by sampling and the reaction was stopped when the content of raw (3-chloro-2-fluorophenyl)methanol was ≤ 1%. After completion of the reaction, the mixture was left to stratify. The organic layer (dichloromethane layer) was separated and the dichloromethane was recovered by simple distillation. Finally, vacuum distillation of the remaining oil layer gave 46.1 g of 3-chloro-2-fluorobenzaldehyde with 97.5% product purity and 91% yield.
261723-30-2
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85070-48-0
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Yield:85070-48-0 91%
Reaction Conditions:
with sodium hypochlorite;2,2,6,6-Tetramethyl-1-piperidinyloxy free radical;sodium hydrogencarbonate in dichloromethane at 0 - 5; for 1 h;Temperature;
Steps:
29 Preparation of 2-fluoro-3-chlorobenzaldehyde
1L four-necked flask, 36.3 g of sodium hydrogencarbonate, 500 g of dichloromethane, 0.5 g of ΤΕΜΡO(jiān), and the mixture was cooled to 0 to 5 ° C with stirring, 50 g of 2-fluoro-3-chlorobenzyl alcohol and 100 g of dichloromethane were added dropwise, and then add the sodium hypochlorite solution 230g, drop after the insulation reaction 1 h, sampling control, raw materials ≤ 1%, stop the reaction, standing stratification, the oil layer of simple distillation of dichloromethane recovery, and then vacuum distillation that 2-fluoro-3-chlorobenzaldehyde 46.1 g, content 97.5%, yield 91%.
References:
CN104529729,2016,B Location in patent:Paragraph 0087; 0088
6574-97-6
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85070-48-0
266 suppliers
$10.00/5g
94087-40-8
183 suppliers
$10.00/5g
85070-48-0
266 suppliers
$10.00/5g