Ammonia → tert-Butyl 2,9-diazaspiro(5.5)undecane-9-carboxylate

HRID 1848430노트

반응식

HRID 1848430 반응식
[CH:1]([C:3]1([CH2:16][CH2:17][CH3:18])[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][CH2:4]1)=O.[NH3:19]>CO.[Ni]>[CH2:8]1[C:3]2([CH2:16][CH2:17][CH2:18][NH:19][CH2:1]2)[CH2:4][CH2:5][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:7]1

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 58017246Tert-butyl 4-formyl-4-propylpiperidine-1-carboxylate

생성물 1

HCID 46912008tert-Butyl 2,9-diazaspiro(5.5)undecane-9-carboxylate

시약·촉매·용매 2

HCID 887Methanol용매HCID 935Nickel용매

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온도
110 °C

실험 절차

Tert-butyl 4-formyl-4-propylpiperidinecarboxylate (30 g) was dissolved in a saturated solution of ammonia in methanol, and 15 g of Raney Ni was added. The reaction mixture was heated to 110° C. at 80 atmospheres pressure in a 2 L high-pressure autoclave. The mixture was filtered to remove the catalyst and the filtrate was concentrated to give residue which was purified by column chromatography to afford tert-butyl 3,8-diazaspiro[5,5]undecane-3-carboxylate.

후처리

  1. additionwas added
  2. filtrationThe mixture was filtered
  3. customto remove the catalyst
  4. concentrationthe filtrate was concentrated
  5. customto give residue which
  6. customwas purified by column chromatography

출처 및 근거

ORD 기록
ord-ce111ee4dfe144ac8dbaf8064ec80bcf
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952166B2

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