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

HRID 1750143노트

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HRID 1750143 반응식
[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]

참가 물질

5

반응물 2

HCID 6577Chloroacetyl chlorideHCID 72652-Amino-4-chlorophenol

생성물 1

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

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-3c91bc869c2b4b2fa6983f505711757f
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09156822B2

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