HCID 4736943、化合物 → HCID 44236229、化合物

HRID 1951286ノート

反応式

HRID 1951286 の反応式
[CH:1]1([C:4]2[CH:20]=[C:7]3[N:8]=[CH:9][CH:10]=[C:11]([S:12][C:13]4[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][CH:14]=4)[N:6]3[N:5]=2)[CH2:3][CH2:2]1.Cl[C:22]1[C:31]2[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=2)[C:25]([C:32]2[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][CH:33]=2)=[N:24][N:23]=1>CC(O)(C)C.C(Cl)Cl>[Cl:38][C:35]1[CH:34]=[CH:33][C:32]([C:25]2[C:26]3[C:31](=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:22]([NH:19][C:16]3[CH:15]=[CH:14][C:13]([S:12][C:11]4[N:6]5[N:5]=[C:4]([CH:1]6[CH2:3][CH2:2]6)[CH:20]=[C:7]5[N:8]=[CH:9][CH:10]=4)=[CH:18][CH:17]=3)=[N:23][N:24]=2)=[CH:37][CH:36]=1

参加物

5

反応物 2

HCID 4736943HCID 4736943、化合物HCID 670171844-(2-Cyclopropylpyrazolo[1,5-a]pyrimidin-7-ylthio)benzenamine

生成物 1

HCID 44236229HCID 44236229、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6386tert-Butanol溶媒

反応条件

温度
100 °C

実験手順

A resealable tube charged with a mixture of 4-(2-cyclopropylpyrazolo[1,5-a]pyrimidin-7-ylthio)benzenamine (100 mg, 0.354 mmol) and 1-chloro-4-(4-chlorophenyl)phthalazine (97 mg, 0.354 mmol) in tBuOH (2 mL) was heated to 100° C. After 3 hrs, the mixture was cooled to RT, diluted with CH2Cl2, and washed with water and brine. After drying the organic fraction with sodium sulfate, the solvent was removed in vacuo. The residue was purified by silica gel chromatography using 20-90% Hexanes:EtOAc to afford 4-(4-chlorophenyl)-N-(4-(2-cyclopropylpyrazolo[1,5-a]pyrimidin-7-ylthio)phenyl)phthalazin-1-amine. MS: Found M+H+=521.2.

後処理

  1. temperaturethe mixture was cooled to RT
  2. washwashed with water and brine
  3. dry with materialAfter drying the organic fraction with sodium sulfate
  4. customthe solvent was removed in vacuo
  5. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-344c65bda8ec4a27afdda6cfed6eacfb
出典データセット
uspto-grants-2013_03
特許番号
US08404694B2

反応ノート

読み込み中…