2-Chloro-6,7-dimethoxy-4-quinazolinamine → HCID 20473808、化合物

HRID 2295733ノート

反応式

HRID 2295733 の反応式
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([Cl:16])[N:3]=1.[C:17]([N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)(=[O:21])/[CH:18]=[CH:19]/[CH3:20]>C(O)CC(C)C>[OH2:12].[ClH:16].[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([N:25]2[CH2:26][CH2:27][N:22]([C:17](=[O:21])/[CH:18]=[CH:19]/[CH3:20])[CH2:23][CH2:24]2)[N:3]=1

参加物

4

反応物 2

HCID 902352-Chloro-6,7-dimethoxy-4-quinazolinamineHCID 58756641-(Piperazin-1-yl)but-2-en-1-one

生成物 1

HCID 20473808HCID 20473808、化合物収率 90%

試薬・触媒・溶媒 1

HCID 31260Isoamyl Alcohol溶媒

実験手順

To 80 ml of isopentanol were added 4.55 g of 4-amino-2-chloro-6,7-dimethoxyquinazoline and 3.4 g of 1-crotonoylpiperazine; the resulting mixture was then refluxed for 1.5 hours. At the end of this time, the hot reaction mixture was filtered. The filtrate was cooled and the crystals which resulted were collected by filtration and then recrystallized from ethanol to give 3.52 g of the desired hydrochloride hydrate of Compound No. 1 in the form of colourless crystals melting at 255°-256° C. (with decomposition):

後処理

  1. temperaturethe resulting mixture was then refluxed for 1.5 hours
  2. filtrationAt the end of this time, the hot reaction mixture was filtered
  3. temperatureThe filtrate was cooled
  4. customthe crystals which resulted
  5. filtrationwere collected by filtration
  6. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-57021342419c40b6857ab907e9de6161
出典データセット
uspto-grants-1984_01
特許番号
US04426382

反応ノート

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