Cyclopropylamine → HCID 178491237、化合物

HRID 732106

反応式

HRID 732106 の反応式
Cl.C(O[C:5](=[NH:14])[C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][CH:7]=1)C.[CH:15]1([NH2:18])[CH2:17][CH2:16]1>C(Cl)Cl>[CH:15]1([NH:18][C:5](=[NH:14])[C:6]2[CH:7]=[CH:8][C:9]([O:12][CH3:13])=[CH:10][CH:11]=2)[CH2:17][CH2:16]1

参加物

4

反応物 2

HCID 69828CyclopropylamineHCID 12270046Ethyl 4-methoxybenzimidate hydrochloride

生成物 1

HCID 178491237HCID 178491237、化合物収率 82%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4-methoxy-benzimidic acid ethyl ester hydrochloride (1.25 g, 5.8 mmol), DCM (5 ml) and cyclopropylamine (0.92 ml, 13.3 mmol) were mixed. After stirring at r.t for 3 h, the reaction mixture was concentrated in-vacuo. The residue was treated with cold aq. sodium hydroxide (1M) and extracted with EA. The combined organic phase was washed with water and brine, dried (Na2SO4), filtered and concentrated in-vacuo, to isolate the title compound (0.90 g, 82%). 1H-NMR: 7.64 (d, 2H), 6.90 (d, 2H), 5.3 (bs, 2H), 3.85 (s, 3H), 2.59 (m, 1H), 0.84 (m, 2H), 0.62 (m, 2H).

後処理

  1. concentrationthe reaction mixture was concentrated in-vacuo
  2. additionThe residue was treated with cold aq. sodium hydroxide (1M)
  3. extractionextracted with EA
  4. washThe combined organic phase was washed with water and brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in-vacuo

出典と根拠

ORDレコード
ord-7fad59dcafca4665b83f4718518a4c68
出典データセット
uspto-grants-2009_09
特許番号
US07585881B2

関連ノート

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