ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrochloric Acid → 2-(3-Hydroxypropylthio)-4,5-bis-(p-methoxyphenyl)-thiazole

HRID 544657
ノート
印刷プレビュー

反応式

HRID 544657 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:13]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)[S:12][C:11](=[S:22])[N:10]=2)=[CH:5][CH:4]=1.[H-].[Na+].Br[CH2:26][CH2:27][CH2:28][OH:29].Cl>CN(C)P(=O)(N(C)C)N(C)C>[OH:29][CH2:28][CH2:27][CH2:26][S:22][C:11]1[S:12][C:13]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)=[C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[N:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 123083-Bromo-1-propanolHCID 24758Sodium hydrideHCID 132096564,5-Bis-(p-methoxyphenyl)-thiazoline-2-thione

生成物 1

HCID 204583792-(3-Hydroxypropylthio)-4,5-bis-(p-methoxyphenyl)-thiazole

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide
溶媒

実験手順

5.0 g of 4,5-bis-(p-methoxyphenyl)-thiazoline-2-thione are dissolved in 50 ml of hexamethylphosphoric acid triamide under nitrogen at 45°, 0.73 g of 50% strength sodium hydride suspension (in mineral oil, de-oiled with hexane) is added in portions and the mixture is stirred at room temperature for 1 hour. 2.22 g of 3-bromopropanol are then added dropwise. The mixture is then stirred at room temperature for 90 minutes, poured into a mixture of 400 ml of ice-water and 20 ml of 2 N hydrochloric acid, extracted by stirring twice with 100 ml of ethyl acetate each time, washed twice with 100 ml of water each time, dried over sodium sulphate and concentrated by evaporation under reduced pressure. The oily crude product is dissolved in 30 ml of toluene, and chromatographed over a column of 30 g of silica gel with toluene as eluant. The 800-1200 ml fractions are combined, concentrated to dryness by evaporation and dried for 3 hours at 0.01 mbar. Analytically pure 2-(3-hydroxypropylthio)-4,5-bis-(p-methoxyphenyl)-thiazole is obtained in the form of a pale yellow oil, Rf value 0.25 (silica gel thin layer/toluene:ethyl acetate 3:1).

後処理

  1. stirringThe mixture is then stirred at room temperature for 90 minutes
  2. extractionextracted
  3. stirringby stirring twice with 100 ml of ethyl acetate each time
  4. washwashed twice with 100 ml of water each time
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated by evaporation under reduced pressure
  7. dissolutionThe oily crude product is dissolved in 30 ml of toluene
  8. customchromatographed over a column of 30 g of silica gel with toluene as eluant
  9. concentrationconcentrated to dryness by evaporation
  10. customdried for 3 hours at 0.01 mbar

出典と根拠

ORDレコード
ord-6eb20d3ccfd54dcdbcf5e9f5fd9e2da4
出典データセット
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04451471

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート