4-Aminophenol → 4-(4-(4-Methoxyphenyl)phthalazin-1-ylamino)phenol hydrochloride

HRID 1013653노트

반응식

HRID 1013653 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.[Cl:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13]([C:20]2[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=2)=[N:12][N:11]=1.C(O)(CC)C>C(OCC)C>[ClH:9].[CH3:27][O:26][C:23]1[CH:22]=[CH:21][C:20]([C:13]2[C:14]3[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:10]([NH:1][C:2]3[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=3)=[N:11][N:12]=2)=[CH:25][CH:24]=1

참가 물질

5

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온도
100 °C

실험 절차

4-Aminophenol (340 mg, 3.1 mmol), 1-chloro-4-(4-methoxyphenyl)phthalazine (837 mg, 3.1 mmol), and sec-butanol (12 mL, 3.1 mmol) were combined in a resealable tube and heated to 100° C. overnight. The reaction progress was monitored by LCMS, and upon completion, the orange reaction was cooled diluted with diethyl ether. The resulting precipitate was filtered and washed with diethyl ether, and the solid was dried in vacuo to provide 4-(4-(4-methoxyphenyl)phthalazin-1-ylamino)phenol hydrochloride (1.17 g, 100% yield) as an orange solid. MS [M+H]=344.0. Calc'd for C19H21N5O: 343.13.

후처리

  1. customupon completion, the orange reaction
  2. temperaturewas cooled
  3. filtrationThe resulting precipitate was filtered
  4. washwashed with diethyl ether
  5. customthe solid was dried in vacuo

출처 및 근거

ORD 기록
ord-019b8483707642eaa568ddbd73ce5d97
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981891B2

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