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2-Chloro-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one → 2-Ethyl-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one

HRID 925566
ノート
印刷プレビュー

反応式

HRID 925566 の反応式
Cl[C:2]1[N:3]([CH2:28][CH2:29][CH3:30])[C:4](=[O:27])[C:5]2[NH:6][C:7]([C:11]3[CH:12]=[N:13][N:14]([CH2:16][C:17]4[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=4)[CH:15]=3)=[N:8][C:9]=2[N:10]=1.[CH2:31]([Mg]Br)[CH3:32]>O1CCOCC1.[Cl-].[Zn+2].[Cl-].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:31]([C:2]1[N:3]([CH2:28][CH2:29][CH3:30])[C:4](=[O:27])[C:5]2[NH:6][C:7]([C:11]3[CH:12]=[N:13][N:14]([CH2:16][C:17]4[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=4)[CH:15]=3)=[N:8][C:9]=2[N:10]=1)[CH3:32]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 668032942-Chloro-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-oneHCID 178418443HCID 178418443、化合物

生成物 1

HCID 469133792-Ethyl-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one収率 10%

試薬・触媒・溶媒 3

HCID 3007855Zincchloride触媒
HCID 178418397
HCID 178418397、化合物
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
50 °C

実験手順

To a solution of 2-Chloro-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one (0.1 g, 0.239 mmol) in dioxane (5 ml) under argon was added ethyl magnesium bromide (0.05 g, 1.146 mmol, 1M solution) and 1M zinc chloride (0.031 g, 2.39 mmol, 1M). To this solution Pd(PPh3)4 (0.026 g, 0.0239 mmol) was added. The reaction mixture was heated at 50° C. for overnight. The reaction mixture was filtered through celite pad and the solvents were removed under reduced pressure. The residue was purified by column chromatography to obtain 2-Ethyl-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one (0.01 g, 10%) as a white solid.

後処理

  1. filtrationThe reaction mixture was filtered through celite pad
  2. customthe solvents were removed under reduced pressure
  3. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-0e21690cdb3849b0bc62b54c5036184b
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09284316B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート