HCID 4736943, 화합물 → HCID 44236229, 화합물

HRID 1951286노트

반응식

HRID 1951286 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 44236229HCID 44236229, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6386tert-Butanol용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-344c65bda8ec4a27afdda6cfed6eacfb
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404694B2

반응 노트

불러오는 중…