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Hydrochloric Acid → 1-(4-Phenyl-1,3-thiazol-2-yl)piperazine

HRID 2262988
ノート
印刷プレビュー

反応式

HRID 2262988 の反応式
[C:1]1([C:7]2[N:8]=[C:9]([N:12]3[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14][CH2:13]3)[S:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.C(OCC)C>C(OCC)(=O)C>[C:1]1([C:7]2[N:8]=[C:9]([N:12]3[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]3)[S:10][CH:11]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 68777857Tert-butyl 4-(4-phenyl-1,3-thiazol-2-yl)piperazine-1-carboxylate

生成物 1

HCID 7124681-(4-Phenyl-1,3-thiazol-2-yl)piperazine収率 80.8%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

tert-Butyl 4-(4-phenyl-1,3-thiazol-2-yl)piperazine-1-carboxylate (691 mg, 2.00 mmol) was dissolved in ethyl acetate (50 ml), and a solution of 4 N hydrogen chloride in ethyl acetate (11 ml) was added thereto, followed by stirring at room temperature for 1 hour and half. Diethyl ether (20 ml) was poured to the reaction mixture, and a solid was separated by filtration, which was dissolved in an aqueous 1 N sodium hydroxide solution (7 ml). Water was poured to the reaction mixture, and the resulting solution was extracted with chloroform. The extract was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to give 396 mg (80.8%) of the desired product as an oil.

後処理

  1. customa solid was separated by filtration, which
  2. dissolutionwas dissolved in an aqueous 1 N sodium hydroxide solution (7 ml)
  3. additionWater was poured to the reaction mixture
  4. extractionthe resulting solution was extracted with chloroform
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-7589fb7cb62749a891620c5bbd18c510
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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