Acetic Acid → 2-{4-[5-(1,1,1,3,3,3-Hexafluoro-2-hydroxypropan-2-yl)-4-propylpyridin-2-yl]piperazin-1-yl}ethyl acetate

HRID 1038512노트

반응식

HRID 1038512 반응식
[F:1][C:2]([F:28])([F:27])[C:3]([C:9]1[CH:10]=[N:11][C:12]([N:18]2[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][OH:26])[CH2:20][CH2:19]2)=[CH:13][C:14]=1[CH2:15][CH2:16][CH3:17])([OH:8])[C:4]([F:7])([F:6])[F:5].N1C=CC=CC=1.[C:35](O)(=[O:37])[CH3:36].CO>ClCCl>[C:35]([O:26][CH2:25][CH2:24][N:21]1[CH2:22][CH2:23][N:18]([C:12]2[CH:13]=[C:14]([CH2:15][CH2:16][CH3:17])[C:9]([C:3]([OH:8])([C:4]([F:7])([F:6])[F:5])[C:2]([F:27])([F:1])[F:28])=[CH:10][N:11]=2)[CH2:19][CH2:20]1)(=[O:37])[CH3:36]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 887MethanolHCID 1049PyridineHCID 866471781,1,1,3,3,3-Hexafluoro-2-{6-[4-(2-hydroxyethyl)piperazin-1-yl]-4-propylpyridin-3-yl}propan-2-ol

생성물 1

HCID 866471772-{4-[5-(1,1,1,3,3,3-Hexafluoro-2-hydroxypropan-2-yl)-4-propylpyridin-2-yl]piperazin-1-yl}ethyl acetate수율 36%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1,1,1,3,3,3-Hexafluoro-2-{6-[4-(2-hydroxyethyl)piperazin-1-yl]-4-propylpyridin-3-yl}propan-2-ol (208 mg, 0.501 mol) was dissolved in dichloromethane (2.5 mL), added pyridine (121 μL, 1.50 mmol) and anhydrous acetic acid (142 μL, 1.50 mmol) under ice-cold conditions, and the mixture was stirred at room temperature for 3 hours. The reaction solution was added methanol, stirred at room temperature for 0.5 hours. The reaction solution was concentrated in vacuo, extracted with chloroform. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The title compound (247 mg) was obtained as a red-brown oil.

후처리

  1. stirringstirred at room temperature for 0.5 hours
  2. concentrationThe reaction solution was concentrated in vacuo
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-dab76b4c5c5d4da2b96dd1aed965a859
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08551985B2

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