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

HRID 1065363
ノート
印刷プレビュー

反応式

HRID 1065363 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b0eba3fd16854d37b234589fb94a54f7
出典データセット
uspto-grants-1982_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04329347

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート