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

HRID 1591614ノート

反応式

HRID 1591614 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5aa63f1536244118a4bc754b9e4f4b53
出典データセット
uspto-grants-2007_11
特許番号
US07291616B2

反応ノート

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