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

HRID 1752248노트

반응식

HRID 1752248 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 10942334Sodium Methoxide촉매HCID 887Methanol용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-7a774b49d8e74e64984cf04a03c9c462
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09163003B2

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