Ammonium Chloride → tert-Butyl (2R,5S)-4-(3-tert-butoxy-4-cyanophenyl)-2,5-dimethylpiperazine-1-carboxylate

HRID 1445466ノート

反応式

HRID 1445466 の反応式
F[C:2]1[CH:3]=[C:4]([N:10]2[C@@H:15]([CH3:16])[CH2:14][N:13]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[C@H:12]([CH3:24])[CH2:11]2)[CH:5]=[CH:6][C:7]=1[C:8]#[N:9].[CH3:25][C:26]([CH3:29])([O-:28])[CH3:27].[K+].[Cl-].[NH4+]>C1COCC1>[C:26]([O:28][C:2]1[CH:3]=[C:4]([N:10]2[C@@H:15]([CH3:16])[CH2:14][N:13]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[C@H:12]([CH3:24])[CH2:11]2)[CH:5]=[CH:6][C:7]=1[C:8]#[N:9])([CH3:29])([CH3:27])[CH3:25]

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 23665647Potassium tert-butoxideHCID 86601755HCID 86601755、化合物

生成物 1

HCID 86601756tert-Butyl (2R,5S)-4-(3-tert-butoxy-4-cyanophenyl)-2,5-dimethylpiperazine-1-carboxylate収率 30.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Into 20 ml of THF was dissolved 3.12 g of tert-butyl (2R,5S)-4-(3-fluoro-4-cyanophenyl)-2,5-dimethylpiperazine-1-carboxylate, and then 1.40 g of potassium tert-butoxide was added thereto, followed by heating under refluxing overnight. A saturated ammonium chloride aqueous solution was added to the reaction solution, followed by extraction with chloroform. After the organic layer was dried over anhydrous sodium sulfate, the solvent was removed by evaporation to obtain 1.11 g of the title compound.

後処理

  1. temperatureby heating
  2. temperatureunder refluxing overnight
  3. extractionfollowed by extraction with chloroform
  4. dry with materialAfter the organic layer was dried over anhydrous sodium sulfate
  5. customthe solvent was removed by evaporation

出典と根拠

ORDレコード
ord-4ebaceab336a4b169833b18a0da61e2b
出典データセット
uspto-grants-2010_02
特許番号
US07666873B2

反応ノート

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