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

2,6-Lutidine → 5-(Benzyloxy)-1-(phenylsulfonyl)-1H-indole-4-carbaldehyde

HRID 2423116
노트
인쇄 미리보기

반응식

HRID 2423116 반응식
Br[C:2]1[C:10]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[CH:5][N:6]2[S:19]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)(=[O:21])=[O:20].C(C([Sn])=C(CCCC)CCCC)CCC.N1C(C)=CC=CC=1C.I([O-])(=O)(=O)=O.[Na+].[O:57]1CCOC[CH2:58]1>C1(C)C=CC=CC=1.O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O=[Os](=O)(=O)=O>[CH2:12]([O:11][C:10]1[CH:9]=[CH:8][C:7]2[N:6]([S:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)(=[O:21])=[O:20])[CH:5]=[CH:4][C:3]=2[C:2]=1[CH:58]=[O:57])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 79372,6-LutidineHCID 312751,4-Dioxane2회HCID 23667635Sodium periodateHCID 53438229Tri(butyl)vinyltinHCID 67240891HCID 67240891, 화합물2회

생성물 1

HCID 866182505-(Benzyloxy)-1-(phenylsulfonyl)-1H-indole-4-carbaldehyde

시약·촉매·용매

4
HCID 30318Osmium Tetroxide촉매HCID 178418476HCID 178418476, 화합물촉매2회HCID 962Water용매HCID 1140Toluene용매

실험 절차

To a warm solution of 4-bromo-5-benzyloxy-1-(phenylsulfonyl)-1H-indole (Intermediate 3, 4.74 g, 10.7 mmol) in toluene (100 mL) was added tributylvinyltin (6.80 g, 21.4 mmol) and Pd(PPh3)2Cl2 (0.37 g, 0.50 mmol). The solution was heated at reflux for two hours and more Pd(PPh3)2Cl2 (0.20 g, 0.30 mmol) was added and the reaction mixture was refluxed overnight. A teaspoon of silica gel was added and the mixture was filtered through a pad of silica gel. The solvent was removed under reduced pressure and the resulting oil was triturated with petroleum ether to give a semicrystalline mass (3.6 g) that was dissolved in dioxane (110 mL) and 2,6-lutidine (2.00 g, 18.7 mmol) and OsO4 (0.24 g, 0.94 mmol) were added. The mixture was stirred at room temperature for five minutes. To the dark solution was added a solution of sodium periodate (8.02 g, 37.5 mmol) in water (35 mL) and the resulting suspension was stirred for 30 minutes. More dioxane (40 mL) was added and the mixture was filtered. The filtrate was evaporated to give a dark red oil. The crude product was purified by flash chromatography on silica gel using petroleum ether/EtOAc 90:10 followed by 80:20 as eluent to give the title compound (2.44 g) as a yellow solid. MS m/z 392 [M+H]+.

후처리

  1. temperatureThe solution was heated
  2. temperatureat reflux for two hours
  3. temperaturethe reaction mixture was refluxed overnight
  4. additionA teaspoon of silica gel was added
  5. filtrationthe mixture was filtered through a pad of silica gel
  6. customThe solvent was removed under reduced pressure
  7. customthe resulting oil was triturated with petroleum ether
  8. customto give a semicrystalline mass (3.6 g) that
  9. stirringthe resulting suspension was stirred for 30 minutes
  10. filtrationthe mixture was filtered
  11. customThe filtrate was evaporated
  12. customto give a dark red oil
  13. customThe crude product was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-fa01a6276d934b79916361bab09e829c
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07960374B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트