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[1-(2,4-dimethoxy-benzyl)-4,4-dimethyl-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-yl]-carbamic acid tert-butyl ester → HCID 69491024, 화합물

HRID 852014
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HRID 852014 반응식
[C:1]([O:5][C:6](=[O:29])[NH:7][CH:8]1[C:14]([CH3:16])([CH3:15])[CH:13]=[CH:12][CH2:11][N:10]([CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][C:19]=2[O:26][CH3:27])[C:9]1=[O:28])([CH3:4])([CH3:3])[CH3:2]>CO.[Pd]>[C:1]([O:5][C:6](=[O:29])[NH:7][CH:8]1[C:14]([CH3:16])([CH3:15])[CH2:13][CH2:12][CH2:11][N:10]([CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][C:19]=2[O:26][CH3:27])[C:9]1=[O:28])([CH3:2])([CH3:3])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 69492432[1-(2,4-dimethoxy-benzyl)-4,4-dimethyl-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-yl]-carbamic acid tert-butyl ester

생성물 1

HCID 69491024HCID 69491024, 화합물수율 84.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

[1-(2,4-Dimethoxy-benzyl)-4,4-dimethyl-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-yl]-carbamic acid tert-butyl ester (260 mg, 0.64 mmol) was dissolved in methanol (10 ml). Palladium on charcoal (30 mg, 10%) was added and the mixture was hydrogenated at room temperature for 90 minutes. The catalyst was filtered off and the filtrate was evaporated. The residue was purified by flash chromatography (heptane/ethyl acetate=1:1) to yield 220 mg (84%) of [1-(2,4-dimethoxy-benzyl)-4,4-dimethyl-2-oxo-azepan-3-yl]-carbamic acid tert-butyl ester as a colourless oil; MS: m/e=407.4 (MH+).

후처리

  1. filtrationThe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. customThe residue was purified by flash chromatography (heptane/ethyl acetate=1:1)

출처 및 근거

ORD 기록
ord-8813226ffd2e4d3e82ca942c7350cfed
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253158B2

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