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

Methanol → 1-(2-Hydroxyethoxy)-2-(2-hydroxyethyl)-3-(tert-butyldiphenylsilyloxy)-propane

HRID 1107014
노트
인쇄 미리보기

반응식

HRID 1107014 반응식
[O:1]=[O+][O-].[CH2:4]([O:7][CH2:8][CH:9]([CH2:29][CH:30]=C)[CH2:10][O:11][Si:12]([C:25]([CH3:28])([CH3:27])[CH3:26])([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)C=C.N#N.[BH4-].[Na+].[CH3:36][OH:37]>C(OCC)(=O)C.CCCCCC>[OH:37][CH2:36][CH2:4][O:7][CH2:8][CH:9]([CH2:29][CH2:30][OH:1])[CH2:10][O:11][Si:12]([C:25]([CH3:28])([CH3:26])[CH3:27])([C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 887MethanolHCID 947NitrogenHCID 24823OzoneHCID 4311764Sodium borohydrideHCID 187904481-(2-Propene-1-oxy)-2-(2-propene-1-yl)-3-(tert-butyldiphenylsilyloxy)-propane

생성물 1

HCID 187904721-(2-Hydroxyethoxy)-2-(2-hydroxyethyl)-3-(tert-butyldiphenylsilyloxy)-propane수율 72%

시약·촉매·용매 1

HCID 21226206Ethyl acetate hexane용매

실험 절차

Ozone was bubbled through a -78 ° C. methanol (500 mL) solution of diene, 1-(2-propene-1-oxy)-2-(2-propene-1-yl)-3-(tert-butyldiphenylsilyloxy)-propane, (7.41 g, 18.80 mmol). After the disappearance of the starting material (TLC, 25% ethyl acetate/hexane), the reaction mixture was purged with N2 and sodium borohydride (2.13 g, 56.30 mmol) was added. The reaction was warmed to room temperature. After 12 hours, the reaction was concentrated. The white residue was quenched with water, and extracted with ethyl acetate (100 mL×3). The combined organic phase was washed with brine, dried, and concentrated under reduced pressure to give a residue. The residue was eluted through a short silica gel column with ethyl acetate/hexane (10% to 50% ethyl acetate gradient) and evaporation of the eluting solvent gave the 1,7-diol, 1-(2-hydroxyethoxy)-2-(2-hydroxyethyl)-3-(tert-butyldiphenylsilyloxy)-propane (5.48 g, 72% yield). Rf =0.21 (50% ethyl acetate in hexane). NMR.

후처리

  1. additionwas added
  2. concentrationthe reaction was concentrated
  3. customThe white residue was quenched with water
  4. extractionextracted with ethyl acetate (100 mL×3)
  5. washThe combined organic phase was washed with brine
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. customto give a residue
  9. washThe residue was eluted through a short silica gel column with ethyl acetate/hexane (10% to 50% ethyl acetate gradient) and evaporation of the eluting solvent

출처 및 근거

ORD 기록
ord-97144e313d214bf5940ea0ab9d89dd94
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06057440

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트