Ammonium Chloride → 2-(3-(4-(4-Methoxybenzoyl)piperidin-1-yl)-2-oxopyrrolidin-1-yl)acetimidamide hydrochloride

HRID 1752248ノート

反応式

HRID 1752248 の反応式
[CH3:1][O:2][C:3]1[CH:25]=[CH:24][C:6]([C:7]([CH:9]2[CH2:14][CH2:13][N:12]([CH:15]3[CH2:19][CH2:18][N:17]([CH2:20][C:21]#[N:22])[C:16]3=[O:23])[CH2:11][CH2:10]2)=[O:8])=[CH:5][CH:4]=1.[Cl-:26].[NH4+:27]>CO.C[O-].[Na+]>[ClH:26].[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]([CH:9]2[CH2:10][CH2:11][N:12]([CH:15]3[CH2:19][CH2:18][N:17]([CH2:20][C:21](=[NH:27])[NH2:22])[C:16]3=[O:23])[CH2:13][CH2:14]2)=[O:8])=[CH:24][CH:25]=1

参加物

5

反応物 2

HCID 25517Ammonium ChlorideHCID 893757962-(3-(4-(4-Methoxybenzoyl)piperidin-1-yl)-2-oxopyrrolidin-1-yl)acetonitrile

生成物 1

HCID 893757462-(3-(4-(4-Methoxybenzoyl)piperidin-1-yl)-2-oxopyrrolidin-1-yl)acetimidamide hydrochloride収率 101.3%

試薬・触媒・溶媒 2

HCID 10942334Sodium Methoxide触媒HCID 887Methanol溶媒

実験手順

To a solution of 2-(3-(4-(4-methoxybenzoyl)piperidin-1-yl)-2-oxopyrrolidin-1-yl)acetonitrile (690 mg, 2.0 mmol) in methanol (15 mL) was added sodium methoxide (0.046 mL, 0.20 mmol, 25%) and the mixture was stirred at ambient temperature for 2 h. Ammonium chloride (120 mg, 2.3 mmol) was added and the mixture was stirred at ambient temperature for 60 h. The reaction mixture was concentrated in vacuo, ethyl acetate in heptane (40%) was added, stirred at ambient temperature for 1 h then filtrated. the resulting solid was washed with ether to give a pale solid (800 mg, 100% yield). MS m/z 342.4 (M+1), retention time 0.79

後処理

  1. stirringthe mixture was stirred at ambient temperature for 60 h
  2. concentrationThe reaction mixture was concentrated in vacuo, ethyl acetate in heptane (40%)
  3. additionwas added
  4. stirringstirred at ambient temperature for 1 h
  5. filtrationthen filtrated
  6. washthe resulting solid was washed with ether

出典と根拠

ORDレコード
ord-7a774b49d8e74e64984cf04a03c9c462
出典データセット
uspto-grants-2015_10
特許番号
US09163003B2

反応ノート

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