Sodium Bicarbonate → 4-Chloro-2-methoxymethyl-6-[4-(3-trifluoromethyl-pyridin-2-yl)-piperazin-1-yl]-pyrimidine

HRID 230938노트

반응식

HRID 230938 반응식
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([CH2:9][O:10][CH3:11])[N:3]=1.[F:12][C:13]([F:27])([F:26])[C:14]1[C:15]([N:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)=[N:16][CH:17]=[CH:18][CH:19]=1.C(=O)(O)[O-].[Na+]>CCO>[Cl:8][C:6]1[CH:7]=[C:2]([N:23]2[CH2:24][CH2:25][N:20]([C:15]3[C:14]([C:13]([F:27])([F:12])[F:26])=[CH:19][CH:18]=[CH:17][N:16]=3)[CH2:21][CH2:22]2)[N:3]=[C:4]([CH2:9][O:10][CH3:11])[N:5]=1

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 27777861-[3-(Trifluoromethyl)pyridin-2-yl]piperazineHCID 534381214,6-Dichloro-2-(methoxymethyl)pyrimidine

생성물 1

HCID 577610444-Chloro-2-methoxymethyl-6-[4-(3-trifluoromethyl-pyridin-2-yl)-piperazin-1-yl]-pyrimidine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Combine 4,6-dichloro-2-methoxymethyl-pyrimidine (800 mg, 4.14 mmol), 1-(3-trifluoromethyl-pyridin-2-yl)-piperazine (960 mg, 4.14 mmol), sodium bicarbonate (500 mg), and EtOH (50 mL). Reflux for 4 hours, let cool to room temperature, vacuum filter, and evaporate the mother liquor. Purify the residue by column chromatography eluting with 20:1 DCM/MeOH to obtain 4-chloro-2-methoxymethyl-6-[4-(3-trifluoromethyl-pyridin-2-yl)-piperazin-1-yl]-pyrimidine as a white solid.

후처리

  1. temperatureReflux for 4 hours
  2. filtrationvacuum filter
  3. customevaporate the mother liquor
  4. customPurify the residue by column chromatography
  5. washeluting with 20:1 DCM/MeOH

출처 및 근거

ORD 기록
ord-b3d76deded3a44e890edb71f8f971faf
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566712B2

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