Dichloromethane → 2-chloro-N-methyl-5-nitrobenzamide

HRID 1435745노트

반응식

HRID 1435745 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4](Cl)=[O:5].Cl.CN.ClCCl.[CH2:20]([N:22](CC)CC)C>C(OCC)(=O)C>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([NH:22][CH3:20])=[O:5]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 117637Benzoyl chloride, 2-chloro-5-nitro-HCID 6364545Methylamine hydrochloride

생성물 1

HCID 27951452-chloro-N-methyl-5-nitrobenzamide

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 2-chloro-5-nitro-benzoyl chloride (502 mg, 2.3 mmol), methylamine hydrochloride (213 mg, 3.1 mmol), dichloromethane (10 ml), and triethylamine (0.84 ml, 6.0 mmol) was stirred for 60 hours. The mixture was treated with ethyl acetate (25 ml). The solution was washed with a mixture of saturated aqueous sodium chloride solution and 1 M hydrochloric acid (1:1, 2×20 ml), washed with aqueous sodium carbonate solution (1 M, 20 ml), dried over sodium sulfate, and concentrated under reduced pressure to provide 2-chloro-N-methyl-5-nitro-benzamide.

후처리

  1. washThe solution was washed with a mixture of saturated aqueous sodium chloride solution and 1 M hydrochloric acid (1:1, 2×20 ml)
  2. washwashed with aqueous sodium carbonate solution (1 M, 20 ml)
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-39e6f89178bf45799ebf142316df145b
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618968B2

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