Trifluoroacetic acid → (4-Morpholin-4-ylmethyl-phenyl)piperazin-1-yl-methanone

HRID 560992ノート

反応式

HRID 560992 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:28])[C:15]2[CH:20]=[CH:19][C:18]([CH2:21][N:22]3[CH2:27][CH2:26][O:25][CH2:24][CH2:23]3)=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl.C([O-])(O)=O.[Na+]>[N:22]1([CH2:21][C:18]2[CH:17]=[CH:16][C:15]([C:14]([N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)=[O:28])=[CH:20][CH:19]=2)[CH2:23][CH2:24][O:25][CH2:26][CH2:27]1

参加物

5

反応物 2

HCID 6422Trifluoroacetic acid2 回HCID 592181854-(4-Morpholin-4-ylmethyl-benzoyl)piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 59218186(4-Morpholin-4-ylmethyl-phenyl)piperazin-1-yl-methanone

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

A solution of 4-(4-morpholin-4-ylmethyl-benzoyl)-piperazine-1-carboxylic acid tert-butyl ester (1.163 g) in CH2Cl2 (10 mL) was treated with trifluoroacetic acid (˜4 mL). After 30 min, additional trifluoroacetic acid (5 mL) was added, and the mixture was stirred for a further 2 h. The mixture was diluted with diluted with saturated aquoues NaHCO3 and extracted with CH2Cl2. The organic layer was dried (Na2SO4) and concentrated. The residue was purified by column chromatography (SiO2) to yield the title compound.

後処理

  1. additionThe mixture was diluted
  2. extractionextracted with CH2Cl2
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography (SiO2)

出典と根拠

ORDレコード
ord-34365dd70b7d4d7e8b977cf9f6272dd1
出典データセット
uspto-grants-2011_11
特許番号
US08063206B2

反応ノート

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