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Potassium tert-butoxide → 5-(2,4-Dimethoxy-benzyl)-7-oxo-2-phenyl-4,5,6,7-tetrahydro-thiazolo[4,5-c]pyridine-6-carboxylic acid ethyl ester

HRID 642278
ノート
印刷プレビュー

反応式

HRID 642278 の反応式
C([O:3][C:4]([C:6]1[S:10][C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:8][C:7]=1[CH2:17][N:18]([CH2:25][C:26]1[CH:31]=[CH:30][C:29]([O:32][CH3:33])=[CH:28][C:27]=1[O:34][CH3:35])[CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])=O)C.CC(C)([O-])C.[K+]>C1COCC1>[CH2:23]([O:22][C:20]([CH:19]1[N:18]([CH2:25][C:26]2[CH:31]=[CH:30][C:29]([O:32][CH3:33])=[CH:28][C:27]=2[O:34][CH3:35])[CH2:17][C:7]2[N:8]=[C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[S:10][C:6]=2[C:4]1=[O:3])=[O:21])[CH3:24]
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

4

反応物 2

HCID 23665647Potassium tert-butoxideHCID 684272284-{[(2,4-Dimethoxy-benzyl)-ethoxycarbonylmethyl-amino]-methyl}-2-phenyl-thiazole-5-carboxylic acid ethyl ester

生成物 1

HCID 684267715-(2,4-Dimethoxy-benzyl)-7-oxo-2-phenyl-4,5,6,7-tetrahydro-thiazolo[4,5-c]pyridine-6-carboxylic acid ethyl ester収率 102.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-78 °C

実験手順

A yellow solution of 4-{[(2,4-dimethoxy-benzyl)-ethoxycarbonylmethyl-amino]-methyl}-2-phenyl-thiazole-5-carboxylic acid ethyl ester (5.60 g, 0.01 mol) in THF (45 mL) was added 1 M potassium tert-butoxide (KOtBu) in THF (24.7 mL, 0.02 mmol) at −78° C., a dark red suspension quickly appeared. The mixture was stirred at −78° C. for 20 min, warmed to room temperature and stirred at that temperature for 2 h before it was quenched with aqueous ammonium chloride, extracted with ethyl acetate. The organic layer was washed with water, brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give 5-(2,4-dimethoxy-benzyl)-7-oxo-2-phenyl-4,5,6,7-tetrahydro-thiazolo[4,5-c]pyridine-6-carboxylic acid ethyl ester as a yellow oil (4.63 g). It was dissolved in dichloromethane (40 mL) and thionyl chloride (1.12 mL, 0.02 mmol) was added drop wise. The mixture was stirred at room temperature for 3.5 h before it was quenched with saturated sodium bicarbonate, extracted with dichloromethane. The organic layer was washed with water, brine, dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and dichloromethane to give the title compound as a yellow solid (2.74 g): 1H NMR (CDCl3, 200 MHz): δ=11.52 (s, 1H), 9.00 (s, 1H), 8.13 (m, 2H), 7.55 (m, 3H), 4.58 (q, J=7.0 Hz, 2H), 1.53 (t, J=7.0 Hz, 3H); MS: (+) m/z 301.0 (M+1).

後処理

  1. temperaturewarmed to room temperature
  2. stirringstirred at that temperature for 2 h before it
  3. customwas quenched with aqueous ammonium chloride
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with water, brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-77f2c20a004a40cc86af8509da305020
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07696223B2

反応ノート

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