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

HRID 74903ノート

反応式

HRID 74903 の反応式
[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]

参加物

4

反応物 1

HCID 67284864Tert-butyl 2-cyano-4,4-difluoropiperidine-1-carboxylate2 回

生成物 1

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

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒2 回

実験手順

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 (46PSI). 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.

後処理

  1. additioncharged into a parr shaker
  2. customwas subject to hydrogenation conditions overnight on the parr shaker (46PSI)
  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

出典と根拠

ORDレコード
ord-593840bea670413cbb3d58b918e1f8d6
出典データセット
uspto-grants-2014_09
特許番号
US08829007B2

反応ノート

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