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

HRID 637983
ノート
印刷プレビュー

反応式

HRID 637983 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

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

生成物 1

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

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-c3f542636fcb434aa952b6bc152e2cf4
出典データセット
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04559348

反応ノート

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