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Water → N-1,2-Benzisoxazol-3-yl-4-(4-phenyl-1,3-thiazol-2-yl)piperidine-1-carboxamide

HRID 2263126
ノート
印刷プレビュー

反応式

HRID 2263126 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([N:10]([C:19]([O:21]CC(Cl)(Cl)Cl)=O)C(OCC(Cl)(Cl)Cl)=O)=[N:2]1.[C:27]1([C:33]2[N:34]=[C:35]([CH:38]3[CH2:43][CH2:42][NH:41][CH2:40][CH2:39]3)[S:36][CH:37]=2)[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1.C(N(C(C)C)CC)(C)C.O>CS(C)=O>[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([NH:10][C:19]([N:41]2[CH2:40][CH2:39][CH:38]([C:35]3[S:36][CH:37]=[C:33]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[N:34]=3)[CH2:43][CH2:42]2)=[O:21])=[N:2]1
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 962WaterHCID 81531DiisopropylethylamineHCID 242618344-Phenyl-2-(piperidin-4-yl)thiazoleHCID 86625471Bis(2,2,2-trichloroethyl) 1,2-benzisoxazol-3-ylimidodicarbonate

生成物 1

HCID 68780004N-1,2-Benzisoxazol-3-yl-4-(4-phenyl-1,3-thiazol-2-yl)piperidine-1-carboxamide収率 47.5%

試薬・触媒・溶媒 1

HCID 679
Dimethyl Sulfoxide
溶媒

実験手順

A solution of bis(2,2,2-trichloroethyl) 1,2-benzisoxazol-3-ylimidodicarbonate (277 mg, 0.573 mmol), 4-(4-phenyl-1,3-thiazol-2-yl)piperidine (280 mg, 1.15 mmol) and diisopropylethylamine (0.0998 ml, 0.573 mmol) in dimethylsulfoxide (3 ml) was stirred at 70° C. for 12 hours, the reaction mixture was poured into water 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 recrystallized from a mixed solvent of hexane and ethyl acetate to obtain the desired product (110 mg, 47.4%) as a solid.

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 recrystallized from a mixed solvent of hexane and ethyl acetate

出典と根拠

ORDレコード
ord-44351b327c31443882eb0586c432e152
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07851473B2

反応ノート

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