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

Methyl iodide → (4R)-4,5-Dihydro-2-(methylthio)-4-thiazolemethanol

HRID 1734506
ノート
印刷プレビュー

反応式

HRID 1734506 の反応式
[OH:1][CH2:2][C@@H:3]1[CH2:7][S:6][C:5]([SH:8])=[N:4]1.[CH:9](N(C(C)C)CC)(C)C.CI>CO>[OH:1][CH2:2][C@@H:3]1[CH2:7][S:6][C:5]([S:8][CH3:9])=[N:4]1
参加物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 6328Methyl iodideHCID 81531DiisopropylethylamineHCID 178521049HCID 178521049、化合物2 回

生成物 1

HCID 22862349(4R)-4,5-Dihydro-2-(methylthio)-4-thiazolemethanol収率 59%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a mixture solution of 4.88 g of 4(R)-hydroxymethyl-2-mercapto-1,3-thiazoline [Compound (5)] and 22.8 ml of diisopropylethylamine in 65 ml of dry methanol was added 14.00 g of methyl iodide under refluxing condition, and the reaction mixture was refluxed for hour. After removal of the solvent under reduced pressure, the resulting residue was dissolved in ethyl acetate and the organic layer was washed with saturated sodium bicarbonate solution, water and saturated saline solution and dried over magnesium sulfate. The solvent was removed under reduced pressure and the resulting residue was purified by silica gel column chromatography (chloroform-acetone) to give 3.14 g (59%) of 4(R)-hydroxymethyl-2-methylthio-1,3-thiazoline [Compound (6)].

後処理

  1. temperatureunder refluxing condition
  2. temperaturethe reaction mixture was refluxed for hour
  3. customAfter removal of the solvent under reduced pressure
  4. dissolutionthe resulting residue was dissolved in ethyl acetate
  5. washthe organic layer was washed with saturated sodium bicarbonate solution, water and saturated saline solution
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was removed under reduced pressure
  8. customthe resulting residue was purified by silica gel column chromatography (chloroform-acetone)

出典と根拠

ORDレコード
ord-2e57b04df3084e9f98c0f822bd41f0c2
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05534510

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