Tert-butyl 2-cyano-4,4-difluoropiperidine-1-carboxylate → Tert-butyl 2-(aminomethyl)-4,4-difluoropiperidine-1-carboxylate

HRID 526927

반응식

HRID 526927 반응식
[C:1]([CH:3]1[CH2:8][C:7]([F:10])([F:9])[CH2:6][CH2:5][N:4]1[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])#[N:2]>[Ni].CO>[NH2:2][CH2:1][CH:3]1[CH2:8][C:7]([F:10])([F:9])[CH2:6][CH2:5][N:4]1[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12]

참가 물질

4

반응물 1

HCID 67284864Tert-butyl 2-cyano-4,4-difluoropiperidine-1-carboxylate2회

생성물 1

HCID 67286116Tert-butyl 2-(aminomethyl)-4,4-difluoropiperidine-1-carboxylate

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매2회

실험 절차

Raney nickel (0.36 mL, 5.40 mmol) was washed with MeOH (2×) and charged into a parr shaker. A solution of tert-butyl 2-cyano-4,4-difluoro-piperidine-1-carboxylate, 13h, (1.33 g, 5.40 mmol) in methanol (50 mL). The reaction mixture was subject to hydrogenation conditions overnight on the parr shaker (46 PSI). The mixture was filtered through celite and washed thoroughly with CH2Cl2. All volatiles were removed at reduced pressure and the crude material was used without further purification.

후처리

  1. additioncharged into a parr shaker
  2. customwas subject to hydrogenation conditions overnight on the parr shaker (46 PSI)
  3. filtrationThe mixture was filtered through celite
  4. washwashed thoroughly with CH2Cl2
  5. customAll volatiles were removed at reduced pressure
  6. customthe crude material was used without further purification

출처 및 근거

ORD 기록
ord-ce5a6db3e68947f1b1ab5a97a09433dc
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09345708B2

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