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

Methyl iodide → HCID 86658011, 화합물

HRID 70654
노트
인쇄 미리보기

반응식

HRID 70654 반응식
[H-].[Na+].[C:3]([C:7]1[CH:12]=[CH:11][C:10](/[C:13](/[C:32]2[CH:37]=[CH:36][C:35]([CH:38]([OH:40])[CH3:39])=[C:34]([O:41][CH3:42])[N:33]=2)=[CH:14]\[C@@H:15]2[N:19]([CH2:20][C:21]3[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[CH:23][C:22]=3[O:29][CH3:30])[C:18](=[O:31])[CH2:17][CH2:16]2)=[CH:9][CH:8]=1)([CH3:6])([CH3:5])[CH3:4].[C:43](=[S:45])=[S:44].[CH3:46]I>O1CCCC1.O>[C:43]([S:45][CH3:46])(=[S:44])[O:40][CH:38]([C:35]1[C:34]([O:41][CH3:42])=[N:33][C:32](/[C:13](/[C:10]2[CH:11]=[CH:12][C:7]([C:3]([CH3:4])([CH3:5])[CH3:6])=[CH:8][CH:9]=2)=[CH:14]/[C@H:15]2[CH2:16][CH2:17][C:18](=[O:31])[N:19]2[CH2:20][C:21]2[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[CH:23][C:22]=2[O:29][CH3:30])=[CH:37][CH:36]=1)[CH3:39]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6328Methyl iodideHCID 6348Carbon DisulfideHCID 24758Sodium hydrideHCID 67399360HCID 67399360, 화합물

생성물 1

HCID 86658011HCID 86658011, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

Sodium hydride (22 mg, 60% in oil) was added to a solution of (5R)-5-{(E)-2-(4-tert-butylphenyl)-2-[5-(1-hydroxyethyl)-6-methoxypyridin-2-yl]ethenyl}-1-(2,4-dimethoxybenzyl)pyrrolidin-2-one (100 mg) in tetrahydrofuran (2 mL) under ice-cooling, and the mixture was stirred at the same temperature for 15 minutes. The reaction solution was warmed to room temperature and carbon disulfide (66.7 μL) was added, followed by stirring for 30 minutes. Methyl iodide (68.5 μL) was added and the mixture was stirred for 3.5 hours. Water was added to the reaction solution, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1→1:1) to give O-[1-(6-{(E)-1-(4-tert-butylphenyl)-2-[(2R)-1-(2,4-dimethoxybenzyl)-5-oxopyrrolidin-2-yl]ethenyl}-2-methoxypyridin-3-yl)ethyl] S-methyl carbonodithioate as a colorless oil (109 mg).

후처리

  1. temperaturecooling
  2. stirringby stirring for 30 minutes
  3. stirringthe mixture was stirred for 3.5 hours
  4. extractionfollowed by extraction with chloroform
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. customafter which the solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1→1:1)

출처 및 근거

ORD 기록
ord-b9b5f7c360c04693889890bd96412fb1
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822503B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트