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

Diisobutylaluminum hydride → [3-Phenyl-1-(toluene-4-sulfonyl)-1H-indol-2-yl]methanol

HRID 242843
노트
인쇄 미리보기

반응식

HRID 242843 반응식
C([O:3][C:4]([C:6]1[N:7]([S:21]([C:24]2[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=2)(=[O:23])=[O:22])[C:8]2[C:13]([C:14]=1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[CH:12][CH:11]=[CH:10][CH:9]=2)=O)C.CC(C[AlH]CC(C)C)C>C1(C)C=CC=CC=1>[C:15]1([C:14]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[N:7]([S:21]([C:24]3[CH:25]=[CH:26][C:27]([CH3:30])=[CH:28][CH:29]=3)(=[O:22])=[O:23])[C:6]=2[CH2:4][OH:3])[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14487Diisobutylaluminum hydrideHCID 681575273-Phenyl-1-(toluene-4-sulfonyl)-1H-indole-2-carboxylic acid ethyl ester

생성물 1

HCID 68156952[3-Phenyl-1-(toluene-4-sulfonyl)-1H-indol-2-yl]methanol수율 85.5%

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
-78 °C

실험 절차

To a stirred solution of 3-phenyl-1-(toluene-4-sulfonyl)-1H-indole-2-carboxylic acid ethyl ester (3.24 g, 7.72 mmol) in toluene (40 mL) cooled to −78° C. and under a nitrogen atmosphere was added 1.0M DIBAL-H in toluene (23.2 mL, 23.2 mmol). The reaction mixture was stirred at −78° C. for 15 min and then at −10° C. for 30 min. After re-cooling to −78° C., the reaction mixture was quenched with water (20 mL) and then allowed to warm to RT. The mixture was partitioned between EtOAc and 1.0M HCl and the aqueous phase was extracted with additional EtOAc (×3). The combined organic layers were washed with water, then dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 30-100% DCM in pentane) affording [3-Phenyl-1-(toluene-4-sulfonyl)-1H-indol-2-yl]methanol as a white foam (2.49 g, 85%). LCMS: RT 4.77 min [M+Na]+ 400.1.

후처리

  1. waitat −10° C. for 30 min
  2. temperatureAfter re-cooling to −78° C.
  3. customthe reaction mixture was quenched with water (20 mL)
  4. temperatureto warm to RT
  5. customThe mixture was partitioned between EtOAc and 1.0M HCl
  6. extractionthe aqueous phase was extracted with additional EtOAc (×3)
  7. washThe combined organic layers were washed with water
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated in vacuo
  10. customThe resulting residue was purified by column chromatography (Si—PCC, gradient 30-100% DCM in pentane)

출처 및 근거

ORD 기록
ord-050e22efc04f470a85222958940614ed
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08653089B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트