Dichloromethane → (2,6-Dichlorophenyl)methyl acetate

HRID 1692111

反応式

HRID 1692111 の反応式
ClCCl.[Cl:4][C:5]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:6]=1[CH2:7][OH:8].[C:14](OC(=O)C)(=[O:16])[CH3:15]>CN(C)C1C=CN=CC=1.C(N(CC)CC)C>[Cl:4][C:5]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:6]=1[CH2:7][O:8][C:14](=[O:16])[CH3:15]

参加物

6

反応物 3

HCID 6344DichloromethaneHCID 7918Acetic Anhydride2 回HCID 27156Benzenemethanol, 2,6-dichloro-

生成物 1

HCID 261530(2,6-Dichlorophenyl)methyl acetate

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 8471Triethylamine溶媒2 回

反応条件

温度
5 °C

実験手順

Add 500 mL of dichloromethane to 100 g of 2,6-dichlorobenzyl alcohol followed by 117 mL of triethylamine. Cool the solution to 5° C. and add 65 mL of acetic anhydride. After 2.5 hr at room temperature, add another 10 mL of acetic anhydride, 20 mL of triethylamine and 0.5 g of 4-dimethylaminopyridine. Wash the organic layer with 1N HCl followed by saturated aqueous sodium bicarbonate and brine. Dry the organic layer (sodium sulfate) and evaporate to afford 131.5 g of the titled compound as an oil.

後処理

  1. washWash the organic layer with 1N HCl
  2. dry with materialDry the organic layer (sodium sulfate)
  3. customevaporate

出典と根拠

ORDレコード
ord-459be403d19f41e198d4c744d78b0cf8
出典データセット
uspto-grants-2012_04
特許番号
US08153807B2

関連ノート

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