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Hydrochloric Acid → 7-Benzylamino-5-methyl-1H-pyrazolo[4,3-b]pyridine

HRID 637983
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반응식

HRID 637983 반응식
Cl[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]2[CH:9]=[N:10][NH:11][C:3]=12.Cl.C(=O)([O-])[O-].[Na+].[Na+].[CH2:19]([NH2:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>>[CH2:19]([NH:26][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]2[CH:9]=[N:10][NH:11][C:3]=12)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 7504BenzylamineHCID 10340Sodium CarbonateHCID 116798717-Chloro-5-methyl-1H-pyrazolo[4,3-b]pyridine

생성물 1

HCID 202548677-Benzylamino-5-methyl-1H-pyrazolo[4,3-b]pyridine

실험 절차

7-Chloro-5-methyl-1H-pyrazolo[4,3-b]pyridine (1 g) and benzylamine (30 ml) were heated under reflux for 6 h. The benzylamine was removed in vacuo to yield an oily solid which was digested with 20% hydrochloric acid. The digest was basified with 10% sodium carbonate solution to yield two phases. The solid in the aqueous phase was filtered off to yield the product (0.71 g). The remaining oily phase was extracted with boiling chloroform (3×20 ml) and the extract dried (MgSO4) and evaporated to yield a second crop of product (0.54 g). The combined solids (1.25 g, 91%) were recrystallised from ethanol/petroleum ether to yield the 7-benzylamino-compound as white crystals m.p. 205°-206°.

후처리

  1. temperatureunder reflux for 6 h
  2. customThe benzylamine was removed in vacuo
  3. customto yield an oily solid which
  4. customto yield two phases
  5. filtrationThe solid in the aqueous phase was filtered off

출처 및 근거

ORD 기록
ord-c3f542636fcb434aa952b6bc152e2cf4
출처 데이터셋
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04559348

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