1-Hydroxy-6-methylsulfonylindole → 6-methanesulfonyl-1H-indole

HRID 1371958

반응식

HRID 1371958 반응식
[CH3:1][S:2]([C:5]1[CH:13]=[C:12]2[C:8]([CH:9]=[CH:10][N:11]2O)=[CH:7][CH:6]=1)(=[O:4])=[O:3]>P(OCC)(OCC)OCC.C(OCC)C>[CH3:1][S:2]([C:5]1[CH:13]=[C:12]2[C:8]([CH:9]=[CH:10][NH:11]2)=[CH:7][CH:6]=1)(=[O:4])=[O:3]

참가 물질

4

반응물 1

HCID 7035381-Hydroxy-6-methylsulfonylindole

생성물 1

HCID 27610676-methanesulfonyl-1H-indole

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 31215Triethyl phosphite용매

반응 조건

온도
160 °C

실험 절차

Dissolve 6-Methanesulfonyl-indol-1-ol (5.0 g, 23.7 mmol) in triethyl phosphite (35 ml) and heat at 160° C. for 5 hours. Cool the solution to ambient temperature and dilute with diethyl ether. Wash the ether solution with brine and water followed by drying (sodium sulfate) and reducing to residue. Crystallize the residue from warm ethyl acetate to give the title compound as colorless cubes: mp 149–152° C. MS (ACPI): m/e 196.0 (M+1). Analysis for C9H9NO2S: Calcd: C, 55.37; H, 4.65; N, 7.17; found: C, 55.14; H, 4.71; N, 7.20.

후처리

  1. temperatureCool the solution to ambient temperature
  2. washWash the ether solution with brine and water
  3. dry with materialby drying (sodium sulfate)
  4. customCrystallize the residue
  5. temperaturefrom warm ethyl acetate

출처 및 근거

ORD 기록
ord-d9a31402847d495ba9abaf5773d1d913
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157488B2

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