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1,1-dimethylethyl [(3S)-1-methyl-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-yl]carbamate → (S)-tert-butyl 1-methyl-2-oxoazepan-3-ylcarbamate

HRID 1366609
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HRID 1366609 반응식
[CH3:1][N:2]1[CH2:8][CH:7]=[CH:6][CH2:5][C@H:4]([NH:9][C:10](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])[C:3]1=[O:17].[H][H]>CO.[Pd]>[CH3:1][N:2]1[CH2:8][CH2:7][CH2:6][CH2:5][C@H:4]([NH:9][C:10](=[O:16])[O:11][C:12]([CH3:13])([CH3:15])[CH3:14])[C:3]1=[O:17]
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참가 물질

5

반응물 2

HCID 866369401,1-dimethylethyl [(3S)-1-methyl-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-yl]carbamateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 60110341(S)-tert-butyl 1-methyl-2-oxoazepan-3-ylcarbamate수율 88%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a degassed solution of 1,1-dimethylethyl [(3S)-1-methyl-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-yl]carbamate (Example 94) (680 mg, 2.8 mmol) in MeOH (20 mL) was added 10% Pd/C (100 mg) and the resulting suspension was stirred overnight under a balloon of hydrogen. Filtration of the catalyst and concentration of the filtrate under reduced pressure yielded 1,1-dimethylethyl [(3S)-1-methyl-2-oxohexahydro-1H-azepin-3-yl]carbamate (470 mg, 88%). LCMS: (M−tBut)+: 186.2.

후처리

  1. filtrationFiltration of the catalyst and concentration of the filtrate under reduced pressure

출처 및 근거

ORD 기록
ord-517ae9aae11d4d0c979f97fbb835b2f8
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07893056B2

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