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

Tetrahydrofuran → 1alpha,3beta-Bis(tert-butyldimethylsilyloxy)-17-(3-ethyl-3-hydroxypentyloxymethyl)androsta-5,7,16-triene

HRID 1792203
노트
인쇄 미리보기

반응식

HRID 1792203 반응식
Cl[Ce](Cl)Cl.[CH2:5]([Mg]Br)[CH3:6].[Si:9]([O:16][C@@H:17]1[C@@:34]2([CH3:35])[C:21](=[CH:22][CH:23]=[C:24]3[C@@H:33]2[CH2:32][CH2:31][C@@:29]2([CH3:30])[C@H:25]3[CH2:26][CH:27]=[C:28]2[CH2:36][O:37][CH2:38][CH2:39][C:40](N(C)C)=[O:41])[CH2:20][C@@H:19]([O:45][Si:46]([C:49]([CH3:52])([CH3:51])[CH3:50])([CH3:48])[CH3:47])[CH2:18]1)([C:12]([CH3:15])([CH3:14])[CH3:13])([CH3:11])[CH3:10].[Cl-].[NH4+].O1CC[CH2:57][CH2:56]1>>[Si:9]([O:16][C@@H:17]1[C@@:34]2([CH3:35])[C:21](=[CH:22][CH:23]=[C:24]3[C@@H:33]2[CH2:32][CH2:31][C@@:29]2([CH3:30])[C@H:25]3[CH2:26][CH:27]=[C:28]2[CH2:36][O:37][CH2:38][CH2:39][C:40]([CH2:5][CH3:6])([OH:41])[CH2:56][CH3:57])[CH2:20][C@@H:19]([O:45][Si:46]([C:49]([CH3:52])([CH3:51])[CH3:50])([CH3:48])[CH3:47])[CH2:18]1)([C:12]([CH3:15])([CH3:14])[CH3:13])([CH3:11])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 8028Tetrahydrofuran2회HCID 25517Ammonium ChlorideHCID 161282Cerium trichlorideHCID 673012321alpha,3beta-bis(tert-butyldimethylsilyloxy)-17-(N,N-dimethylaminocarbonylethoxymethyl)androsta-5,7,16-trieneHCID 178418443HCID 178418443, 화합물

생성물 1

HCID 69630501
1alpha,3beta-Bis(tert-butyldimethylsilyloxy)-17-(3-ethyl-3-hydroxypentyloxymethyl)androsta-5,7,16-triene
수율 56%

실험 절차

Tetrahydrofuran (11 ml) was mixed with anhydrous cerous (III) chloride (2.33 g, 9.46 mmol), stirred under nitrogen stream at room temperature for 30 min., cooled with ice, mixed with ethylmagnesium bromide (0.96 mol/l, 9.0 ml, 8.6 mmol) and stirred for 30 min. The reaction solution was mixed with a solution of 1α,3β-bis(tert-butyldimethylsilyloxy)-17-(N,N-dimethylaminocarbonylethoxymethyl)androsta-5,7,16-triene (553 mg, 0.86 mmol) in tetrahydrofuran (11 ml) at 0° C., followed by stirring for 1 hour at the same temperature. The reaction solution was poured into a saturated aqueous ammonium chloride solution, extracted with ethyl acetate (3 times), washed with saturated brine and water, dried over anhydrous magnesium sulfate and evaporated under reduced pressure to remove solvent, giving a reaction mixture containing a ketone body. The thus obtained mixture was again subjected to the same reaction and worked up; the thus obtained residue was purified by column chromatography (hexane:ethyl acetate=5:1) to give the titled compound (317 mg, 56.0%) as a yellow oil.

후처리

  1. temperaturecooled with ice
  2. stirringstirred for 30 min
  3. stirringby stirring for 1 hour at the same temperature
  4. extractionextracted with ethyl acetate (3 times)
  5. washwashed with saturated brine and water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated under reduced pressure
  8. customto remove solvent
  9. customgiving a reaction mixture
  10. customThe thus obtained mixture was again subjected to the same reaction
  11. customthe thus obtained residue was purified by column chromatography (hexane:ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-aa466e4402f844efbbd164d3cf1c23bb
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07074777B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트