N-(5,5-Dimethyl-8-nitro-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)-2-methoxy-acetamide → (5,5-Dimethyl-8-nitro-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)-(2-methoxy-ethyl)-amine

HRID 1687670노트

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HRID 1687670 반응식
[CH3:1][C:2]1([CH3:23])[C:8]2[CH:9]=[CH:10][C:11]([N+:13]([O-:15])=[O:14])=[CH:12][C:7]=2[NH:6][C:5](=O)[CH:4]([NH:17][C:18](=O)[CH2:19][O:20][CH3:21])[CH2:3]1>C1COCC1>[CH3:1][C:2]1([CH3:23])[C:8]2[CH:9]=[CH:10][C:11]([N+:13]([O-:15])=[O:14])=[CH:12][C:7]=2[NH:6][CH2:5][CH:4]([NH:17][CH2:18][CH2:19][O:20][CH3:21])[CH2:3]1

참가 물질

3

반응물 1

HCID 67264613N-(5,5-Dimethyl-8-nitro-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)-2-methoxy-acetamide

생성물 1

HCID 67264406(5,5-Dimethyl-8-nitro-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)-(2-methoxy-ethyl)-amine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
70 °C

실험 절차

A solution of N-(5,5-Dimethyl-8-nitro-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)-2-methoxy-acetamide (0.138 g, 0.43 mmol) in THF (10 mL, 0.1 mol) was treated with 1 M of Borane-THF complex in THF (3 mL). The reaction mixture was heated at 70° C. for 3 hours. The reaction mixture was quenched by the slow dropwise addition of methanol until all bubbling ceased, was concentrated, taken up in CH2Cl2 and washed with water. The organic layer was dried over magnesium sulfate, filtered, and concentrated under reduced pressure.

후처리

  1. customThe reaction mixture was quenched by the slow dropwise addition of methanol until all bubbling
  2. concentrationwas concentrated
  3. washwashed with water
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a1bb30abe8f14ac18e771b09753e12d0
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148391B2

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