Trifluoroacetic acid → Trifluoroacetylpiperazine

HRID 401614

反応式

HRID 401614 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:19])[C:15]([F:18])([F:17])[F:16])[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[F:18][C:15]([F:16])([F:17])[C:14]([N:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1)=[O:19]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 20294522Tert-butyl 4-(2,2,2-trifluoroacetyl)piperazine-1-carboxylate

生成物 1

HCID 7172020Trifluoroacetylpiperazine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of compound 1c (15.15 g, 53.69 mmol) in CH2Cl2 (60 mL) was added trifluoroacetic acid (18 mL) at room temperature. The mixture was stirred at room temperature for 18 h. The solvent was removed by evaporation. Ether (100 mL) was added to the residue. The white solid was collected by filtration, washed with ether, and dried under vacuum. The crude compound 1d was used in the next reaction without further purification. MS m/z (M+H+) 183.1.

後処理

  1. customThe solvent was removed by evaporation
  2. additionEther (100 mL) was added to the residue
  3. filtrationThe white solid was collected by filtration
  4. washwashed with ether
  5. customdried under vacuum
  6. customThe crude compound 1d was used in the next reaction without further purification

出典と根拠

ORDレコード
ord-13a94fe105ab43799c4b132dee85e047
出典データセット
uspto-grants-2014_06
特許番号
US08741887B2

関連ノート

読み込み中…