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Ethanol → 6-(4-Phenylsulfinyl-butoxy)-3,4-dihydro-carbostyril

HRID 1065363
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HRID 1065363 반응식
[C:1]1([S:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]2[CH:14]=[C:15]3[C:20](=[CH:21][CH:22]=2)[NH:19][C:18](=[O:23])[CH2:17][CH2:16]3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(Cl)(Cl)(=O)=[O:25].C(O)C>C(Cl)Cl>[C:1]1([S:7]([CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]2[CH:14]=[C:15]3[C:20](=[CH:21][CH:22]=2)[NH:19][C:18](=[O:23])[CH2:17][CH2:16]3)=[O:25])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 24648Sulfuryl chlorideHCID 248459066-(4-Phenylmercapto-butoxy)-3,4-dihydro-carbostyril

생성물 1

HCID 131383416-(4-Phenylsulfinyl-butoxy)-3,4-dihydro-carbostyril

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
-70 °C

실험 절차

3.3 gm of 6-(4-phenylmercapto-butoxy)-3,4-dihydro-carbostyril were dissolved in 50 ml of methylene chloride, the solution cooled to -70° C., and a solution of 1.5 gm of sulfuryl chloride in 5 ml of methylene chloride was added dropwise. After 15 hours, 20 ml of 95% ethanol were added, and the mixture was heated to room temperature by removing the cooling bath, neutralized with an aqueous sodium carbonate solution. The methylene chloride phase was dried with sodium sulfate, and the solvent was evaporated. The residue was recrystallized from toluene.

후처리

  1. temperaturethe mixture was heated to room temperature
  2. customby removing the cooling bath
  3. dry with materialThe methylene chloride phase was dried with sodium sulfate
  4. customthe solvent was evaporated
  5. customThe residue was recrystallized from toluene

출처 및 근거

ORD 기록
ord-b0eba3fd16854d37b234589fb94a54f7
출처 데이터셋
uspto-grants-1982_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04329347

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