2-[3-(2-Fluorobenzyl)-1H-pyrazolo[4,3-b]pyridin-1-yl]-5-nitropyrimidine-4,6-diamine → HCID 24794429、化合物

HRID 1875456ノート

反応式

HRID 1875456 の反応式
[F:1][C:2]1[CH:28]=[CH:27][CH:26]=[CH:25][C:3]=1[CH2:4][C:5]1[C:9]2=[N:10][CH:11]=[CH:12][CH:13]=[C:8]2[N:7]([C:14]2[N:19]=[C:18]([NH2:20])[C:17]([N+:21]([O-])=O)=[C:16]([NH2:24])[N:15]=2)[N:6]=1>N1C=CC=CC=1.[Pd]>[F:1][C:2]1[CH:28]=[CH:27][CH:26]=[CH:25][C:3]=1[CH2:4][C:5]1[C:9]2=[N:10][CH:11]=[CH:12][CH:13]=[C:8]2[N:7]([C:14]2[N:19]=[C:18]([NH2:20])[C:17]([NH2:21])=[C:16]([NH2:24])[N:15]=2)[N:6]=1

参加物

4

反応物 1

HCID 591778732-[3-(2-Fluorobenzyl)-1H-pyrazolo[4,3-b]pyridin-1-yl]-5-nitropyrimidine-4,6-diamine

生成物 1

HCID 24794429HCID 24794429、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 1049Pyridine溶媒

反応条件

温度
50 °C

実験手順

690 mg (1.42 mmol) of 2-[3-(2-fluorobenzyl)-1H-pyrazolo[4,3-b]pyridin-1-yl]-5-nitropyrimidine-4,6-diamine from example 15A are dissolved in 120 ml of pyridine. 270 mg of 10% palladium on activated carbon are added, and hydrogenation is carried out under a hydrogen pressure of 3.5 bar for 15 h. The catalyst is then filtered off and washed with ethanol. The residue after concentration to dryness is stirred with ethanol at 50° C. and filtered off with suction. 378 mg (76% of theory) of the desired product are obtained. A further 92 mg (18% of theory) of the target compound can be obtained from the filtrate by purifying by preparative HPLC.

後処理

  1. customfor 15 h
  2. filtrationThe catalyst is then filtered off
  3. washwashed with ethanol
  4. concentrationThe residue after concentration to dryness
  5. filtrationfiltered off with suction

出典と根拠

ORDレコード
ord-5a0310e471ef47098f6ad1a28482e1bf
出典データセット
uspto-grants-2012_11
特許番号
US08309551B2

反応ノート

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