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Thiazole → 2-[4-(Pyrid-3-yloxymethyl)-2-phenylbenzoyl]4-ethylthiazole-5-carboxylic acid ethyl ester

HRID 2121197
ノート
印刷プレビュー

反応式

HRID 2121197 の反応式
[CH3:1][O:2][C:3]([C:5]1[S:9][C:8](N)=[N:7][C:6]=1[CH2:11][CH3:12])=[O:4].C[Si](C)(C)[N-][Si](C)(C)C.[Li+].[N:23]1[CH:28]=[CH:27][CH:26]=[C:25]([O:29][CH2:30][C:31]2[CH:39]=[CH:38][C:34]([C:35](O)=[O:36])=[C:33]([C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=3)[CH:32]=2)[CH:24]=1.[C:46](N1C=CN=C1)(N1C=CN=C1)=O.[N-]1C=CN=C1.S1C=CN=C1>CN(C=O)C.C1COCC1>[CH2:1]([O:2][C:3]([C:5]1[S:9][C:8]([C:35](=[O:36])[C:34]2[CH:38]=[CH:39][C:31]([CH2:30][O:29][C:25]3[CH:24]=[N:23][CH:28]=[CH:27][CH:26]=3)=[CH:32][C:33]=2[C:40]2[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=2)=[N:7][C:6]=1[CH2:11][CH3:12])=[O:4])[CH3:46]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 9256ThiazoleHCID 682631,1'-CarbonyldiimidazoleHCID 735005Methyl 2-amino-4-ethyl-1,3-thiazole-5-carboxylateHCID 2733832Lithium hexamethyldisilazaneHCID 3386966ImidazolateHCID 234363704-(3-Pyridyloxymethyl)2-phenylbenzoic acid

生成物 1

HCID 53646307
2-[4-(Pyrid-3-yloxymethyl)-2-phenylbenzoyl]4-ethylthiazole-5-carboxylic acid ethyl ester
収率 48.1%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a −12° C. solution in DMF (2 mL) of 2-amino-4-ethylthiazole-5-carboxylic acid methyl ester (80 mg, 0.40 mmol), prepared as described in J. Chem. Soc. Perkin 1, 1982, 154, was added lithium hexamethyldisilazide (1.0 M in THF, 0.76 mL, 0.76 mmol) and the resulting yellow solution was stirred for 30 minutes. In a separate flask 4-(3-pyridyloxymethyl)-2-phenylbenzoic acid (101 mg, 0.33 mmol), prepared as in Example 228D and carbonyldiimidazole (60 mg, 0.37 mmol) were dissolved in THF and stirred for 1 hour. The resulting imidazolide solution was then added to the thiazole solution at −10° C. and the mixture was stirred for 30 minutes. The cold bath was then removed and stirring was continued for 30 minutes. The reaction mixture was quenched with saturated aqueous ammonium chloride and poured into water. The mixture was extracted twice with dichloromethane. The combine organic extracts were dried, filtered and concentrated. The solid residue was recrystallized from ethyl acetate-methanol to give 2-[4-(pyrid-3-yloxymethyl)-2-phenylbenzoyl]4-ethylthiazole-5-carboxylic acid ethyl ester (75 mg).

後処理

  1. stirringstirred for 1 hour
  2. stirringthe mixture was stirred for 30 minutes
  3. customThe cold bath was then removed
  4. stirringstirring
  5. waitwas continued for 30 minutes
  6. customThe reaction mixture was quenched with saturated aqueous ammonium chloride
  7. additionpoured into water
  8. extractionThe mixture was extracted twice with dichloromethane
  9. customThe combine organic extracts were dried
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customThe solid residue was recrystallized from ethyl acetate-methanol

出典と根拠

ORDレコード
ord-87888cd3bf61469b95f5c0919b5eba80
出典データセット
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06693123B2

反応ノート

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