Aluminium lithium hydride → HCID 57748298, 화합물

HRID 906060노트

반응식

HRID 906060 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]2[CH:16]=[CH:15][C:11]([C:12]([NH2:14])=O)=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]2[CH:9]=[CH:10][C:11]([CH2:12][NH2:14])=[CH:15][CH:16]=2)[CH2:4][CH2:3]1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 674037884-(1-Methylpiperidin-4-yl)benzamide

생성물 1

HCID 57748298HCID 57748298, 화합물수율 73.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To an ice cold solution of 4-(1-methylpiperidin-4-yl)benzamide (190 mg, 0.87 mmol) in tetrahydrofuran (5 mL) was added 1.0M lithium aluminum hydride in tetrahydrofuran (1.79 mL, 1.79 mmol) and stirring continued overnight at room temperature. The reaction mixture was quenched by adding sodium sulfate decahydrate until gas evolution ceased. The suspension was filtered through Celite and the filter cake washed with a mixture of ethyl acetate and chloroform (2:1, 50 mL). The filtrate was concentrated to give 4-(1-methylpiperidin-4-yl)benzylamine (130 mg, 71%) as an oil. 1H NMR (400 MHz, CDCl3): 7.23 (dd, 4H), 3.86 (s, 3H), 2.98 (m, 2H), 2.49 (m, 1H), 2.11 (m, 2H), 1.83 (m, 4H).

후처리

  1. customThe reaction mixture was quenched
  2. additionby adding sodium sulfate decahydrate until gas evolution
  3. filtrationThe suspension was filtered through Celite
  4. washthe filter cake washed with a mixture of ethyl acetate and chloroform (2:1, 50 mL)
  5. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-57b5c9593d1646fb824971cc27b5b5a4
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012956B2

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