Triethylamine → 3-chloro-N,N-dimethyl-4-methylamino-benzamide

HRID 1949896ノート

反応式

HRID 1949896 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[NH:11][CH3:12])[C:5](O)=[O:6].C(C1NC=CN=1)([C:15]1[NH:16][CH:17]=CN=1)=O.C(N(CC)CC)C>C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[NH:11][CH3:12])[C:5]([N:16]([CH3:17])[CH3:15])=[O:6]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 5250894Bis-(1H-imidazol-2-YL)-methanoneHCID 230850783-Chloro-4-(methylamino)benzoic acid

生成物 1

HCID 668685293-chloro-N,N-dimethyl-4-methylamino-benzamide

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To 3-chloro-4-methylamino-benzoic acid (387 mg) in dry N. N-dimethylformamide (10 mL) was added carbonyl diimidazole (440 mg). After one hour, dimethylamine. HCl (221 mg) and triethylamine (0.38 mL) were added. The reaction mixture was stirred overnight, then diluted with ethyl acetate, washed with brine, dried (MgSO4) and the solvent removed in vacuo. Purification using flash chromatography yielded 3-chloro-N,N-dimethyl-4-methylamino-benzamide.

後処理

  1. washwashed with brine
  2. dry with materialdried (MgSO4)
  3. customthe solvent removed in vacuo
  4. customPurification

出典と根拠

ORDレコード
ord-a235395cc8164ca7b86592449b534664
出典データセット
uspto-grants-2013_03
特許番号
US08399690B2

反応ノート

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