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

HRID 1445466노트

반응식

HRID 1445466 반응식
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]

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 23665647Potassium tert-butoxideHCID 86601755HCID 86601755, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4ebaceab336a4b169833b18a0da61e2b
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07666873B2

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