Acetic Acid → HCID 21485896、化合物

HRID 1414891ノート

反応式

HRID 1414891 の反応式
Cl[C:2]1[N:11]=[C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:18][CH3:19])[CH:8]=2)[N:3]=1.O.[NH2:21][NH2:22].C(O)(=O)C>C(O)C>[NH:21]([C:2]1[N:11]=[C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:18][CH3:19])[CH:8]=2)[N:3]=1)[NH2:22]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 214859182-Chloro-6-methoxy-4-phenylquinazoline

生成物 1

HCID 21485896HCID 21485896、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 9.7 g of 2-chloro-4-phenyl-6-methoxyquinazoline in 300 ml of ethanol were added 15 ml of hydrazine hydrate and 8 ml of glacial acetic acid and the mixture was refluxed for 5 hours. After the precipitate was filtered off, the filtrate was concentrated in vacuo to give crystals. The crystals were collected by filtration, washed with ethanol, and dried to give 7.8 g of 2-hydrazino-4-phenyl-6-methoxyquinazoline, a part of which was recrystallized from ethanol to give yellow scales, m.p. 151° - 152° C.

後処理

  1. temperaturethe mixture was refluxed for 5 hours
  2. filtrationAfter the precipitate was filtered off
  3. concentrationthe filtrate was concentrated in vacuo
  4. customto give crystals
  5. filtrationThe crystals were collected by filtration
  6. washwashed with ethanol
  7. customdried

出典と根拠

ORDレコード
ord-59bad7b51a1d48c5bf4d06c1f1f26702
出典データセット
uspto-grants-1977_01
特許番号
US04002755

反応ノート

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