Chloroacetyl chloride → 2-Chloro-N-(5-chloro-2-hydroxyphenyl)acetamide

HRID 1750143ノート

反応式

HRID 1750143 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[OH:9].[Cl:10][CH2:11][C:12](Cl)=[O:13]>C(Cl)Cl.N1C=CC=CC=1>[Cl:10][CH2:11][C:12]([NH:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[OH:9])=[O:13]

参加物

5

反応物 2

HCID 6577Chloroacetyl chlorideHCID 72652-Amino-4-chlorophenol

生成物 1

HCID 74542742-Chloro-N-(5-chloro-2-hydroxyphenyl)acetamide収率 55%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a cooled (0° C.) solution of 2-amino-4-chlorophenol (30 g, 209 mmol) in DCM (200 mL) and pyridine (17 mL) was added a solution of chloroacetyl chloride in DCM (23.6 g, 230 mmol in 75 mL). The mixture was allowed to reach rt slowly and was subsequently stirred for 18 h. The precipitate was filtered, washed with DCM, and dried overnight at 50° C. to give crude 2-chloro-N-(5-chloro-2-hydroxyphenyl)acetamide (intermediate 56) (26 g, 55%), as a brown solid which was used in the next step without any further purification.

後処理

  1. customto reach rt
  2. filtrationThe precipitate was filtered
  3. washwashed with DCM
  4. customdried overnight at 50° C.

出典と根拠

ORDレコード
ord-3c91bc869c2b4b2fa6983f505711757f
出典データセット
uspto-grants-2015_10
特許番号
US09156822B2

反応ノート

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