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Potassium Carbonate → 6-Ethynyl-1,3-benzothiazole

HRID 2244115
ノート
印刷プレビュー

反応式

HRID 2244115 の反応式
C(=O)([O-])[O-].[K+].[K+].C[Si]([C:11]#[C:12][C:13]1[CH:21]=[CH:20][C:16]2[N:17]=[CH:18][S:19][C:15]=2[CH:14]=1)(C)C>CO>[C:12]([C:13]1[CH:21]=[CH:20][C:16]2[N:17]=[CH:18][S:19][C:15]=2[CH:14]=1)#[CH:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 231545826-Trimethylsilanylethynylbenzothiazol

生成物 1

HCID 231545886-Ethynyl-1,3-benzothiazole収率 96.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Potassium carbonate (29.7 g) was added to a solution of 6-trimethylsilanylethynylbenzothiazol (45.1 g) in methanol (600 ml), and the mixture was stirred for 1.5 hours at room temperature. The reaction solution was filtered, and then the resultant was washed with methanol and ethyl acetate successively. The filtrate was concentrated, to which water was added, and then extracted with ethyl acetate. The organic layer, which was washed with a brine, was dried over anhydrous magnesium sulfate. After the solvent was evaporated, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1→1:1) to yield 6-ethynylbenzothiazole (30.0 g) as a light yellow solid (mp: 47.5-49.0° C.).

後処理

  1. filtrationThe reaction solution was filtered
  2. washthe resultant was washed with methanol and ethyl acetate successively
  3. concentrationThe filtrate was concentrated, to which water
  4. additionwas added
  5. extractionextracted with ethyl acetate
  6. washThe organic layer, which was washed with a brine
  7. dry with materialwas dried over anhydrous magnesium sulfate
  8. customAfter the solvent was evaporated
  9. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1→1:1)

出典と根拠

ORDレコード
ord-0079baf0a95844538dcdefce8e31c9cd
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07678810B2

反応ノート

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