Hydrochloric Acid → 7-[2-(3-Fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-8-propyl-[1,2,4]triazolo[1,5-c]pyrimidin-2-ol

HRID 916669노트

반응식

HRID 916669 반응식
[F:1][C:2]1[C:3]([C:8]2[N:9]([CH2:13][C:14]3[N:19]=[CH:18][N:17]=[C:16](NN)[C:15]=3[CH2:22][CH2:23][CH3:24])[CH:10]=[CH:11][N:12]=2)=[N:4][CH:5]=[CH:6][CH:7]=1.[NH2:25][C:26]([NH2:28])=[O:27].O.Cl>CN1C(=O)CCC1>[F:1][C:2]1[C:3]([C:8]2[N:9]([CH2:13][C:14]3[N:19]=[CH:18][N:17]4[N:25]=[C:26]([OH:27])[N:28]=[C:16]4[C:15]=3[CH2:22][CH2:23][CH3:24])[CH:10]=[CH:11][N:12]=2)=[N:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 1176UreaHCID 57503304{6-[2-(3-Fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-5-propyl-pyrimidin-4-yl}-hydrazine

생성물 1

HCID 1784393657-[2-(3-Fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-8-propyl-[1,2,4]triazolo[1,5-c]pyrimidin-2-ol

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
160 °C

실험 절차

To the solution of 131 (3.27, 10 mmol) in anhydrous NMP (3.6 mL) under nitrogen is added urea (1.60 g, 26 mmol). The resulting mixture is heated to 160° C. and stirred for 6 hours. On cooling, the reaction mixture is poured into water (80 mL), pH is adjusted to 7 with hydrochloric acid, and the solution is extracted with dichloromethane (50 ml×4). The organic solution is dried with anhydrous sodium sulfate and concentrated to give the crude product 177 as an oil which is used directly in the next step reaction.

후처리

  1. temperatureOn cooling
  2. extractionthe solution is extracted with dichloromethane (50 ml×4)
  3. dry with materialThe organic solution is dried with anhydrous sodium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4cf7ddd6f82947faabb92497b632d52c
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07271170B2

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