Water → 2-(4-{5-[1,1,1,3,3,3-Hexafluoro-2-(4-methoxybenzyloxy)propan-2-yl]-4-propylpyridin-2-yl}piperazin-1-yl)ethyl acetate

HRID 1038513노트

반응식

HRID 1038513 반응식
[C:1]([O:4][CH2:5][CH2:6][N:7]1[CH2:12][CH2:11][N:10]([C:13]2[CH:18]=[C:17]([CH2:19][CH2:20][CH3:21])[C:16]([C:22]([OH:31])([C:27]([F:30])([F:29])[F:28])[C:23]([F:26])([F:25])[F:24])=[CH:15][N:14]=2)[CH2:9][CH2:8]1)(=[O:3])[CH3:2].[C:32](=[O:35])([O-])[O-].[K+].[K+].CO[CH:40](Cl)[C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1.O>CN(C=O)C>[C:1]([O:4][CH2:5][CH2:6][N:7]1[CH2:8][CH2:9][N:10]([C:13]2[CH:18]=[C:17]([CH2:19][CH2:20][CH3:21])[C:16]([C:22]([O:31][CH2:40][C:41]3[CH:46]=[CH:45][C:44]([O:35][CH3:32])=[CH:43][CH:42]=3)([C:23]([F:26])([F:25])[F:24])[C:27]([F:30])([F:28])[F:29])=[CH:15][N:14]=2)[CH2:11][CH2:12]1)(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium Carbonate2회HCID 11062637Methoxybenzyl chloride2회HCID 866471772-{4-[5-(1,1,1,3,3,3-Hexafluoro-2-hydroxypropan-2-yl)-4-propylpyridin-2-yl]piperazin-1-yl}ethyl acetate

생성물 1

HCID 866471792-(4-{5-[1,1,1,3,3,3-Hexafluoro-2-(4-methoxybenzyloxy)propan-2-yl]-4-propylpyridin-2-yl}piperazin-1-yl)ethyl acetate수율 89.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2-{4-[5-(1,1,1,3,3,3-Hexafluoro-2-hydroxypropan-2-yl)-4-propylpyridin-2-yl]piperazin-1-yl}ethyl acetate (211 mg, 0.461 mol) was dissolved in N,N′-dimethylformamide (2.3 mL), and added potassium carbonate (191 mg, 1.38 mmol) at room temperature. Under ice-cold conditions, methoxybenzyl chloride (125 μL, 0.923 mmol) was added, and the mixture was stirred at room temperature overnight. Subsequently, potassium carbonate (96 mg, 0.690 mmol) was further added at room temperature, methoxybenzyl chloride (63 μL, 0.462 mmol) was added under ice-cold conditions, and the mixture was stirred at room temperature for 8 hours. The reaction solution was added water, extracted with chloroform. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The title compound (479 mg) was obtained as a red-brown oil.

후처리

  1. stirringthe mixture was stirred at room temperature for 8 hours
  2. extractionextracted with chloroform
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e9694551891f456dadce016f706eee4b
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08551985B2

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