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HCID 54549910, 화합물 → tert-butyl N-{6-azaspiro[3.4]octan-8-yl}carbamate

HRID 378573
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HRID 378573 반응식
[C:1]([O:5][C:6]([NH:8][CH:9]1[C:13]2([CH2:16][CH2:15][CH2:14]2)[CH2:12][N:11]([C@@H](C2C=CC=CC=2)C)[CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(O)C.[Pd]>[C:1]([O:5][C:6]([NH:8][CH:9]1[C:13]2([CH2:14][CH2:15][CH2:16]2)[CH2:12][NH:11][CH2:10]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 54549910HCID 54549910, 화합물

생성물 1

HCID 19354273tert-butyl N-{6-azaspiro[3.4]octan-8-yl}carbamate수율 102.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

To a solution of 4.1 g of 8-tert-butoxycarbonylamino-6-[1-(R)-phenylethyl]-6-azaspiro[3.4]octane in 60 ml of ethanol there was added 4.5 g of 5% palladium on charcoal (50% wet) and reduction was carried out under a hydrogen atmosphere (H2 pressure: 4 atm.) for 5 hrs. During the reduction, the reaction vessel was warmed by irradiation with a tungsten lamp. At 1 hr. from the beginning of the reduction, 2 g of the same catalyst was further added and the reduction continued for an additional 4 hours at the same condition to total 5 hours. The catalyst was removed by filtration and the solvent was removed under reduced pressure to yield 2.88 g of the titled compound.

후처리

  1. customfor 5 hrs
  2. temperatureDuring the reduction, the reaction vessel was warmed by irradiation with a tungsten lamp
  3. waitthe reduction continued for an additional 4 hours at the same condition to total 5 hours
  4. customThe catalyst was removed by filtration
  5. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-d559ec4571754fc9985ef27eccc5802a
출처 데이터셋
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06031102

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