Hydrochloric Acid → HCID 5329079、化合物

HRID 962616ノート

反応式

HRID 962616 の反応式
[OH-].[Na+].[Br:3][C:4]1[CH:5]=[C:6]([NH:10][C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([NH:21][C:22](=[O:30])/[CH:23]=[CH:24]/[C:25]([O:27]CC)=[O:26])[CH:19]=3)[N:14]=[CH:13][N:12]=2)[CH:7]=[CH:8][CH:9]=1.Cl>C(O)C>[Br:3][C:4]1[CH:5]=[C:6]([NH:10][C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([NH:21][C:22](=[O:30])/[CH:23]=[CH:24]/[C:25]([OH:27])=[O:26])[CH:19]=3)[N:14]=[CH:13][N:12]=2)[CH:7]=[CH:8][CH:9]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 5329080HCID 5329080、化合物

生成物 1

HCID 5329079HCID 5329079、化合物収率 45%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A 2.5 ml portion of 10N aqueous sodium hydroxide was added to 2.3 g of 4-[[4-[(3-bromophenyl)amino]-6-quinazolinyl]amino]-4oxo-(E)-2-butenoic acid ethyl ester (Example 5) in 25 ml of ethanol. After stirring for an hour, 2.1 ml of concentrated hydrochloric acid was added, and the reaction was stirred an additional 2 hours. The resulting solid was recrystallized from n-butanol to give 0.97 g of 4-[[4-[(3-Bromophenyl)amino]-6-quinazolinyl]amino]-4-oxo-(E)-2-butenoic acid: mass spectrum (m/e): M+H 413.

後処理

  1. stirringthe reaction was stirred an additional 2 hours
  2. customThe resulting solid was recrystallized from n-butanol

出典と根拠

ORDレコード
ord-26aec41eef2f4d6e88b4acbf085a593e
出典データセット
uspto-grants-1998_06
特許番号
US05760041

反応ノート

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