Sodium Acetate → HCID 68825906、化合物

HRID 230561ノート

反応式

HRID 230561 の反応式
Cl[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:4]=1[N+:13]([O-:15])=[O:14].[C:16]([O-:19])(=[O:18])[CH3:17].[Na+]>C(O)(=O)C.O>[C:16]([O:19][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:4]=1[N+:13]([O-:15])=[O:14])(=[O:18])[CH3:17]

参加物

5

反応物 2

HCID 517045Sodium AcetateHCID 27757862-Nitro-4-(trifluoromethyl)benzyl chloride

生成物 1

HCID 68825906HCID 68825906、化合物収率 97.9%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

2 g (8.348 mmol) of 1-chloromethyl-2-nitro-4-trifluoromethylbenzene are added, at a temperature in the region of 20° C., under an argon atmosphere, to 20 g (244 mmol) of sodium acetate in solution in 100 cm3 of acetic acid. After stirring for 60 hours at a temperature in the region of 100° C., the reaction mixture is diluted with 200 cm3 of water and then extracted with 2 times 300 cm3 of dichloromethane. The organic phases are combined, washed with 100 cm3 of water, dried over anhydrous magnesium sulfate, filtered, and concentrated to dryness under reduced pressure (2.7 kPa), to give 2.15 g of 2-nitro-4-trifluoromethylbenzyl acetate in the form of an orange oil;

後処理

  1. extractionextracted with 2 times 300 cm3 of dichloromethane
  2. washwashed with 100 cm3 of water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)

出典と根拠

ORDレコード
ord-15a4c2a28a064c979f5cae950ec3a019
出典データセット
uspto-grants-2009_07
特許番号
US07566736B2

反応ノート

読み込み中…