Acetic Acid → Tert-butyl 2-(chloromethyl)-4-oxo-1,3,8-triazaspiro[4.5]dec-1-ene-8-carboxylate

HRID 1013081노트

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HRID 1013081 반응식
[NH2:1][C:2]1([C:15](=[O:17])[NH2:16])[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][CH2:3]1.[Cl:18][CH2:19][C:20](OC)(OC)OC.C(O)(=O)C>>[Cl:18][CH2:19][C:20]1[NH:16][C:15](=[O:17])[C:2]2([CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:12])([CH3:13])[CH3:14])=[O:9])[CH2:4][CH2:3]2)[N:1]=1

참가 물질

4

반응물 3

HCID 176Acetic AcidHCID 1447021,1,1-Trimethoxy-2-chloroethaneHCID 10562199tert-Butyl 4-amino-4-carbamoylpiperidine-1-carboxylate

생성물 1

HCID 57908082Tert-butyl 2-(chloromethyl)-4-oxo-1,3,8-triazaspiro[4.5]dec-1-ene-8-carboxylate수율 67%

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온도
118 °C

실험 절차

1C (0.3M) was added 2-chloro-1,1,1-trimethoxyethane (4.0 equivalents) and acetic acid (2.0 equivalents). The mixture was stirred for 12 hr at 118° C. Solvent was removed under reduced pressure and the residue was purified by crystallization from cold diethyl ether to afford tert-butyl 2-(chloromethyl)-4-oxo-1,3,8-triazaspiro[4.5]dec-1-ene-8-carboxylate (1D, 67%).

후처리

  1. customSolvent was removed under reduced pressure
  2. customthe residue was purified by crystallization from cold diethyl ether

출처 및 근거

ORD 기록
ord-233f9b8f83244ebaa8da77b64ee7e9cf
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981904B2

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