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Water → 1-(6-Methyl-1,3-benzothiazol-2-yl)ethan-1-one

HRID 369102
ノート
印刷プレビュー

反応式

HRID 369102 の反応式
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]2[N:6]=[CH:7][S:8][C:4]=2[CH:3]=1.C([Li])CCC.CN(C)[C:18](=[O:20])[CH3:19].O>C1COCC1>[C:18]([C:7]1[S:8][C:4]2[CH:3]=[C:2]([CH3:1])[CH:10]=[CH:9][C:5]=2[N:6]=1)(=[O:20])[CH3:19]
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 962WaterHCID 31374DimethylacetamideHCID 37454556-methylbenzothiazoleHCID 178418339Butyllithium

生成物 1

HCID 232854001-(6-Methyl-1,3-benzothiazol-2-yl)ethan-1-one収率 47.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 6-methylbenzothiazole (6.1 g, 41 mmol) in anhydrous THF (150 ml) was cooled to -78° C. To the cooled solution was added, with stirring, n-butyl lithium (28.1 ml of 1.6 M n-BuLi-containing hexane solution, 45 mmol) dropwise under nitrogen atmosphere. Further, a solution of N,N-dimethyl acetamide (3.9 g, 45 mmol) in anhydrous THF (70 ml) was added dropwise to the mixture at the same temperature. After completion of the addition, the mixture was stirred for an hour, and then warmed to room temperature. The reaction mixture was poured into water, and then extracted with benzene. The extract was washed with water, dried over magnesium sulfate, and then evaporated. The resulting residual powders were subjected to purification using column chromatography on silica gel (eluant, n-hexane/ethyl acetate=95/5) to afford 2-acetyl-6-methylbenzothiazole (3.7 g, 47%) as a pale yellow powder, together with the starting material (2.5 g).

後処理

  1. additionTo the cooled solution was added
  2. additionAfter completion of the addition
  3. stirringthe mixture was stirred for an hour
  4. extractionextracted with benzene
  5. washThe extract was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated
  8. customThe resulting residual powders were subjected to purification

出典と根拠

ORDレコード
ord-db8239554b494447822630555ccfdd7b
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06136831

反応ノート

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