Tert-butyl 3-(benzyloxy)-1-oxa-8-azaspiro[4.5]decane-8-carboxylate → tert-Butyl 3-hydroxy-1-oxa-8-azaspiro[4.5]decane-8-carboxylate

HRID 2300164

반응식

HRID 2300164 반응식
C([O:8][CH:9]1[CH2:13][C:12]2([CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][CH2:14]2)[O:11][CH2:10]1)C1C=CC=CC=1.[H][H]>O1CCCC1.[C].[Pd]>[OH:8][CH:9]1[CH2:13][C:12]2([CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][CH2:14]2)[O:11][CH2:10]1

참가 물질

5

반응물 2

HCID 22744533Tert-butyl 3-(benzyloxy)-1-oxa-8-azaspiro[4.5]decane-8-carboxylateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 22744549tert-Butyl 3-hydroxy-1-oxa-8-azaspiro[4.5]decane-8-carboxylate수율 89.1%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 8028Tetrahydrofuran용매

실험 절차

6.47 g of tert-butyl 3-(benzyloxy)-1-oxa-8-azaspiro[4.5]decane-8-carboxylate was dissolved in 100 ml tetrahydrofuran, 1.3 g palladium carbon was added thereto, and the mixture was stirred overnight in a hydrogen atmosphere. The catalyst was filtered off from the reaction solution, 1.3 g of palladium carbon was added thereto, and the solution was stirred overnight in a hydrogen atmosphere. The catalyst was filtered off from the reaction solution, 2.6 g of palladium carbon was added thereto, and the solution was stirred overnight in a hydrogen atmosphere at 4.2 atmospheric pressure. The catalyst was filtered off from the reaction solution, the solvent was evaporated, and the resulting residue was purified by silica gel column chromatography (ethyl acetate/methanol) to give 4.27 g of tert-butyl 3-hydroxy-1-oxa-8-azaspiro[4.5]decane-8-carboxylate.

후처리

  1. filtrationThe catalyst was filtered off from the reaction solution, 1.3 g of palladium carbon
  2. additionwas added
  3. filtrationThe catalyst was filtered off from the reaction solution, 2.6 g of palladium carbon
  4. additionwas added
  5. stirringthe solution was stirred overnight in a hydrogen atmosphere at 4.2 atmospheric pressure
  6. filtrationThe catalyst was filtered off from the reaction solution
  7. customthe solvent was evaporated
  8. customthe resulting residue was purified by silica gel column chromatography (ethyl acetate/methanol)

출처 및 근거

ORD 기록
ord-9568fe80ede14ae1be604142cfec6a1f
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06498159B1

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