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

Chloromethyl methyl sulfide → (+)[N-(Benzyloxycarbonyl)morphinan-3-yloxy]methyl methyl sulfide

HRID 1924436
노트
인쇄 미리보기

반응식

HRID 1924436 반응식
[H-].[Na+].[OH:3][C:4]1[CH:5]=[CH:6][C:7]2[CH2:8][C@H:9]3[N:20]([C:21]([O:23][CH2:24][C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)=[O:22])[CH2:19][CH2:18][C@@:15]4([C:16]=2[CH:17]=1)[C@H:10]3[CH2:11][CH2:12][CH2:13][CH2:14]4.[CH3:31][S:32][CH2:33]Cl>CN(P(N(C)C)(N(C)C)=O)C>[CH3:31][S:32][CH2:33][O:3][C:4]1[CH:5]=[CH:6][C:7]2[CH2:8][C@H:9]3[N:20]([C:21]([O:23][CH2:24][C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)=[O:22])[CH2:19][CH2:18][C@@:15]4([C:16]=2[CH:17]=1)[C@H:10]3[CH2:11][CH2:12][CH2:13][CH2:14]4
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 16916Chloromethyl methyl sulfideHCID 24758Sodium hydrideHCID 538511903-hydroxy-N-(benzyloxycarbonyl)morphinan

생성물 1

HCID 67519161(+)[N-(Benzyloxycarbonyl)morphinan-3-yloxy]methyl methyl sulfide수율 26%

시약·촉매·용매 1

HCID 12679Hexamethylphosphoramide용매2회

실험 절차

To Sodium hydride (763 mg of 60% dispersion in mineral oil, 19.1 mmol) in HMPA (15 mL) was added a solution of (+)-3-hydroxy-N-(benzyloxycarbonyl)morphinan (6.00 g, 15.9 mmol) from Example 1 in HMPA (50 mL) at room temperature. The reaction mixture was stirred for 30 min and then chloromethyl methyl sulfide (1.60 mL, 19.1 mmol) was added dropwise. The reaction mixture was stirred vigorously at room temperature overnight. The product was extracted with EtOAc (500 mL). The EtOAc layer was washed with saturated NaHCO3 solution and dried over MgSO4, filtered and evaporated under vacuum to provide the crude product, which was further purified by prep reverse-phase HPLC to afford the title compound (1.78 g, 26%) as a yellow gum.

후처리

  1. stirringThe reaction mixture was stirred vigorously at room temperature overnight
  2. extractionThe product was extracted with EtOAc (500 mL)
  3. washThe EtOAc layer was washed with saturated NaHCO3 solution
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated under vacuum
  7. customto provide the crude product, which
  8. customwas further purified by prep reverse-phase HPLC

출처 및 근거

ORD 기록
ord-50b87131f6e64864906f12ea4d863030
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08178551B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트