o-Chlorophenylacetic acid → HCID 46318635、化合物

HRID 2354097ノート

反応式

HRID 2354097 の反応式
Cl.[CH3:2][NH:3][O:4][CH3:5].[Cl:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH2:13][C:14]([OH:16])=O>ClCCl>[Cl:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH2:13][C:14]([N:3]([O:4][CH3:5])[CH3:2])=[O:16]

参加物

4

反応物 2

HCID 17124o-Chlorophenylacetic acidHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)

生成物 1

HCID 46318635HCID 46318635、化合物収率 93.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
22.5 °C

実験手順

Under ice-cooling, N,O-dimethylhydroxylamine hydrochloride (3.42 g) was added to a mixture of (2-chlorophenyl)acetic acid (3.41 g) and WSCD (2.05 g) in dichloromethane (30 mL). The mixture was stirred at 0-10° C. for an hour and at 20-25° C. for 20 hours, washed with water, dried over magnesium sulfate and concentrated under reduced pressure to give a residue. The residue was purified by silica gel (chromatorex NH) (hexane-AcOEt 50:50 v/v) to give 2-(2-chlorophenyl)-N-methoxy-N-methylacetamide as oil (3.99 g).

後処理

  1. temperatureUnder ice-cooling
  2. washwashed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give a residue
  6. customThe residue was purified by silica gel (chromatorex NH) (hexane-AcOEt 50:50 v/v)

出典と根拠

ORDレコード
ord-17cb3c9219fd4b9da5b47c6816594ab6
出典データセット
uspto-grants-2010_07
特許番号
US07750155B2

反応ノート

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