홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Tert-Butanesulfinamide → t-butyl N-[(1S)-2-[(t-butylsulfinyl)imino]-2-(4-fluorophenyl)-1-methylethyl]carbamate

HRID 1829883
노트
인쇄 미리보기

반응식

HRID 1829883 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[C@@H:9]([NH:11][C:12](=[O:18])[O:13][C:14]([CH3:17])([CH3:16])[CH3:15])[CH3:10])=[CH:4][CH:3]=1.[CH3:20][C:21]([S:24]([NH2:26])=[O:25])([CH3:23])[CH3:22]>>[C:21]([S:24]([N:26]=[C:8]([C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1)[C@@H:9]([NH:11][C:12](=[O:18])[O:13][C:14]([CH3:17])([CH3:16])[CH3:15])[CH3:10])=[O:25])([CH3:23])([CH3:22])[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 3382465Tert-ButanesulfinamideHCID 11265628HCID 11265628, 화합물

생성물 1

HCID 86589064t-butyl N-[(1S)-2-[(t-butylsulfinyl)imino]-2-(4-fluorophenyl)-1-methylethyl]carbamate

실험 절차

The intermediate in Reference Example 5, t-butyl N-[(1S)-2-(4-fluorophenyl)-1-methyl-2-oxoethyl]carbamate and 2-methyl-2-propanesulfinamide were condensed in the presence of a dehydrating agent to give t-butyl N-[(1S)-2-[(t-butylsulfinyl)imino]-2-(4-fluorophenyl)-1-methylethyl]carbamate. 1.0M trimethylaluminum-hexane solution (0.43 mL) was added to the solution of said sulfinylimine compound (80 mg) in toluene (2 mL) at −78° C., and the mixture was stirred for 5 minutes. The obtained solution was dropwise added slowly to 2-fluoro-4-pyridyllithium solution (prepared by the reaction of 4-fluoro-2-bromopyridine (114 mg) and 1.56M butyllithium-hexane solution (0.46 mL) in diethyl ether solvent (3 mL) at −78° C.) at −78° C. Thereafter tetrahydrofuran (3 mL) was added to the reaction mixture, and then the reaction mixture was stirred at −78° C. for 2.5 hours. Saturated sodium chloride aqueous solution was added to the reaction mixture, and temperature of the reaction mixture was raised to room temperature. The obtained reaction mixture was filtered through celite, and then the organic layer of filtrate was dried over anhydrous magnesium sulfate. Magnesium sulfate was removed by filtration, and then the organic solvent was evaporated in vacuo. The obtained residue was purified by silica gel column chromatography (C-300; hexane:ethyl acetate=2:1) to give the optical active t-butyl N-[(1S)-2-[(t-butylsulfinyl)amino]-2-(4-fluorophenyl)-2-(2-fluoro-4-pyridyl)-1-methylethyl]carbamate (49 mg). The product was treated with 4N hydrogen chloride-dioxane solution to give the optical active title diamine (31 mg).

후처리

  1. customcondensed in the presence of a dehydrating agent

출처 및 근거

ORD 기록
ord-5cf3bb93d9484f998a3b0e31b55c3095
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07064142B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트