Water → HCID 68778457、化合物

HRID 2263304ノート

反応式

HRID 2263304 の反応式
Br[C:2]1[S:3][CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([CH3:13])[CH:8]=2)[N:6]=1.[N:14]1([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:13][C:9]1[CH:8]=[C:7]([C:5]2[N:6]=[C:2]([N:17]3[CH2:16][CH2:15][N:14]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:19][CH2:18]3)[S:3][CH:4]=2)[CH:12]=[CH:11][CH:10]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 49758214Thiazole, 2-bromo-4-(3-methylphenyl)-

生成物 1

HCID 68778457HCID 68778457、化合物収率 69.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2-bromo-4-(3-methylphenyl)-1,3-thiazole (2.03 g, 7.99 mmol), tert-butyl piperazine-1-carboxylate (2.98 g, 16.0 mmol) and potassium carbonate (1.10 g, 7.99 mmol) in dimethylformamide (25 ml) was stirred at 120° C. for 12 hours. Water was poured to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with water, and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to give 2.00 g (69.7%) of the desired product as an oil.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1)

出典と根拠

ORDレコード
ord-1a54a1d1dc684fa49ccda91c67d0a653
出典データセット
uspto-grants-2010_12
特許番号
US07851473B2

反応ノート

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