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

Methyl (methylsulfinyl)methyl sulfide → 1-p-Nitrobenzyloxycarbonyl-4-hydroxy-4-methylsulfinylmethylthiomethylpiperidine

HRID 1252233
노트
인쇄 미리보기

반응식

HRID 1252233 반응식
[CH3:1][S:2][CH2:3][S:4]([CH3:6])=[O:5].C([Li])CCC.[N+:12]([C:15]1[CH:31]=[CH:30][C:18]([CH2:19][O:20][C:21]([N:23]2[CH2:28][CH2:27][C:26](=[O:29])[CH2:25][CH2:24]2)=[O:22])=[CH:17][CH:16]=1)([O-:14])=[O:13]>O1CCCC1.CCCCCC.ClCCl.O>[N+:12]([C:15]1[CH:16]=[CH:17][C:18]([CH2:19][O:20][C:21]([N:23]2[CH2:24][CH2:25][C:26]([OH:29])([CH2:1][S:2][CH2:3][S:4]([CH3:6])=[O:5])[CH2:27][CH2:28]2)=[O:22])=[CH:30][CH:31]=1)([O-:14])=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 99129Methyl (methylsulfinyl)methyl sulfideHCID 13292708(4-Nitrophenyl)methyl 4-oxopiperidine-1-carboxylateHCID 178418339Butyllithium

생성물 1

HCID 571340091-p-Nitrobenzyloxycarbonyl-4-hydroxy-4-methylsulfinylmethylthiomethylpiperidine

시약·촉매·용매 4

HCID 962Water용매
HCID 6344
Dichloromethane
용매
HCID 8028Tetrahydrofuran용매2회
HCID 8058Hexane용매

실험 절차

To methyl methylthiomethyl sulfoxide (2.23 g) in dry tetrahydrofuran (10 ml) was added dropwise n-butyl lithium (1.15 g) in dry hexane (11.6 ml) at -60° to -70° C. under nitrogen atmosphere and the mixture was stirred for 20 minutes at the same temperature. Subsequently, 1-p-nitrobenzyloxycarbonyl-4-piperidone (5.0 g) in dry tetrahydrofuran (30 ml) was added dropwise thereto at -55° to -70° C. under nitrogen atmosphere. The reaction mixture was diluted with dichloromethane (200 ml) and water (215 ml), warmed slowly to room temperature, dried over anhydrous sodium sulfate and evaporated to give an oily residue which was then purified by silica gel chromatography to give 1-p-nitrobenzyloxycarbonyl-4-hydroxy-4-methylsulfinylmethylthiomethylpiperidine.

후처리

  1. customat -55° to -70° C.
  2. dry with materialdried over anhydrous sodium sulfate
  3. customevaporated
  4. customto give an oily residue which
  5. customwas then purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-f2e618b6c3ab4ebdb1878a655134e8a7
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04742052

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트