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Ethyl Acetoacetate → Ethyl 2-(2-acetylaminothiazol-4-yl)-4-(2-chloro-4-fluorophenyl)-6-methyl-1,4-dihydro-pyrimidin-5-carboxylate

HRID 1919563
ノート
印刷プレビュー

反応式

HRID 1919563 の反応式
Cl.[C:2]([NH:5][C:6]1[S:7][CH:8]=[C:9]([C:11]([NH2:13])=[NH:12])[N:10]=1)(=[O:4])[CH3:3].[Cl:14][C:15]1[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:16]=1[CH:17]=O.[C:24]([O:30][CH2:31][CH3:32])(=[O:29])[CH2:25][C:26]([CH3:28])=O.C([O-])(=O)C.[Na+]>C(O)C>[C:2]([NH:5][C:6]1[S:7][CH:8]=[C:9]([C:11]2[NH:13][C:26]([CH3:28])=[C:25]([C:24]([O:30][CH2:31][CH3:32])=[O:29])[CH:17]([C:16]3[CH:19]=[CH:20][C:21]([F:23])=[CH:22][C:15]=3[Cl:14])[N:12]=2)[N:10]=1)(=[O:4])[CH3:3]
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 8868Ethyl AcetoacetateHCID 1450242-Chloro-4-fluorobenzaldehydeHCID 517045Sodium AcetateHCID 86640675HCID 86640675、化合物

生成物 1

HCID 59272704Ethyl 2-(2-acetylaminothiazol-4-yl)-4-(2-chloro-4-fluorophenyl)-6-methyl-1,4-dihydro-pyrimidin-5-carboxylate収率 35.5%

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

2 mmol 2-Acetylamino-4-thiazolformamidine hydrochloride, 2 mmol 2-chloro-4-fluorobenzaldehyde, 2 mmol ethyl acetoacetate and 2.2 mmol sodium acetate were reacted under reflux in 10 ml anhydrous ethanol for 20 hr, concentrated, and then ethyl acetate and water were added to separate the layers. The ethyl acetate layer was dried over anhydrous sodium sulfate, and separated by a column chromatography to obtain 0.31 g of a colorless crystal with mp 220-223° C.; 1H-NMR (400 MHz, DMSO-d6) δ 1.01-1.04 (3H, m); 2.13 (3H, s); 2.40-2.42 (3H, d); 3.91-3.97 (2H, m); 5.97 (1H, s); 7.15-7.39 (3H, m); 7.64-7.83 (1H, d); 8.33-8.98 (1H, d); 12.33 (1H, s); MS (EI) 436.0 (M+).

後処理

  1. concentrationconcentrated
  2. additionethyl acetate and water were added
  3. customto separate the layers
  4. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
  5. customseparated by a column chromatography

出典と根拠

ORDレコード
ord-d0988d1ef4624a47b9d4f3ff50068110
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08168642B2

反応ノート

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