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Nitrogen → tert-Butyl 4-amino-3,3-difluoropiperidine-1-carboxylate

HRID 2280375
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HRID 2280375 반응식
N#N.C([NH:10][CH:11]1[CH2:16][CH2:15][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:13][C:12]1([F:25])[F:24])C1C=CC=CC=1>CO.[Pd]>[NH2:10][CH:11]1[CH2:16][CH2:15][N:14]([C:17]([O:19][C:20]([CH3:21])([CH3:22])[CH3:23])=[O:18])[CH2:13][C:12]1([F:25])[F:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 947NitrogenHCID 66710726tert-Butyl 4-(benzylamino)-3,3-difluoropiperidine-1-carboxylate

생성물 1

HCID 56932105tert-Butyl 4-amino-3,3-difluoropiperidine-1-carboxylate

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), tert-butyl 4-(benzylamino)-3,3-difluoropiperidine-1-carboxylate (0.186 g, 0.57 mmol) was dissolved in MeOH (5 mL) and wet Pd/C 10% (50 mg) was added. The flask was purged with H2 gas and the reaction mixture stirred under an H2 atmosphere for 2 h at rt. The reaction mixture was filtered over celite and the cake was washed with MeOH and EA. The filtrate was concentrated under reduced pressure to give tert-butyl 4-amino-3,3-difluoropiperidine-1-carboxylate as a colorless oil. LC-MS-conditions 08: tR=0.49 min; [M-CH3+H]+=222.32.

후처리

  1. customThe flask was purged with H2 gas
  2. filtrationThe reaction mixture was filtered over celite
  3. washthe cake was washed with MeOH and EA
  4. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2aac53795fe049d684178aa48c838a19
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09139524B2

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