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

HRID 1042793노트

반응식

HRID 1042793 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

반응물 3

HCID 4034-AminophenolHCID 6568(+-)-2-ButanolHCID 27723901-Chloro-4-(4-methoxyphenyl)phthalazine

생성물 1

HCID 1363400374-(4-(4-Methoxyphenyl)phthalazin-1-ylamino)phenol hydrochloride수율 100%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

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-b081803c459848febde67b5f8b3f667b
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08557816B2

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