Dodecanoyl chloride → 4-(3-Chloro-phenylamino)-3-(4-[n-dodecanoyl]-piperazin-1-yl)-1h-pyrazolo[3,4-d]pyrimidine

HRID 1068896ノート

反応式

HRID 1068896 の反応式
Cl.Cl.[Cl:3][C:4]1[CH:5]=[C:6]([NH:10][C:11]2[N:16]=[CH:15][N:14]=[C:13]3[NH:17][N:18]=[C:19]([N:20]4[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]4)[C:12]=23)[CH:7]=[CH:8][CH:9]=1.C(=O)([O-])[O-].[K+].[K+].[C:32](Cl)(=[O:44])[CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43]>O.O1CCOCC1>[Cl:3][C:4]1[CH:5]=[C:6]([NH:10][C:11]2[N:16]=[CH:15][N:14]=[C:13]3[NH:17][N:18]=[C:19]([N:20]4[CH2:25][CH2:24][N:23]([C:32](=[O:44])[CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43])[CH2:22][CH2:21]4)[C:12]=23)[CH:7]=[CH:8][CH:9]=1

参加物

6

反応物 3

HCID 8166Dodecanoyl chlorideHCID 11430Potassium CarbonateHCID 211906574-(3-chlorophenylamino)-3-(piperazin-1-yl)-1H-pyrazolo[3,4-d]pyrimidine dihydrochloride

生成物 1

HCID 211907004-(3-Chloro-phenylamino)-3-(4-[n-dodecanoyl]-piperazin-1-yl)-1h-pyrazolo[3,4-d]pyrimidine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

Analogously to Example 26, 100 mg (0.248 mmol) of 4-(3-chloro-phenylamino)-3-(piperazin-1-yl)-1H-pyrazolo[3,4-d]pyrmidine dihydrochloride and 103 mg (0.74 mmol) of potassium carbonate in 10 ml of water are reacted with 81.5 mg (0.37 mmol) of lauric acid chloride in 10 ml of dioxane and extracted. Column chromatography (SiO2; methylene chloride/ethyl acetate/acetic acid=50:50:1) yields 4-(3-chloro-phenylamino)-3-(4-[n-dodecanoyl]-piperazin-1-yl)-1H-pyrazolo[3,4-d]pyrimidine; HPLC: tRet(grad20-100/20)=22.6; FAB-MS: (M+H)+=512.

後処理

  1. extractionextracted

出典と根拠

ORDレコード
ord-d7046b47f4a44631bb7d0d5ecd5bbe49
出典データセット
uspto-grants-2001_06
特許番号
US06251911B1

反応ノート

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