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

HRID 1042793ノート

反応式

HRID 1042793 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b081803c459848febde67b5f8b3f667b
出典データセット
uspto-grants-2013_10
特許番号
US08557816B2

反応ノート

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