Benzenamine, 3-ethynyl- → HCID 16733971、化合物

HRID 2423006ノート

反応式

HRID 2423006 の反応式
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:16][C:17](=[O:19])[CH3:18])=[C:9]([O:12][C:13](=[O:15])[CH3:14])[CH:10]=2)[N:5]=[CH:4][N:3]=1.[C:20]([C:22]1[CH:23]=[C:24]([CH:26]=[CH:27][CH:28]=1)[NH2:25])#[CH:21]>>[ClH:1].[C:20]([C:22]1[CH:23]=[C:24]([NH:25][C:2]2[C:11]3[C:6](=[CH:7][C:8]([O:16][C:17](=[O:19])[CH3:18])=[C:9]([O:12][C:13](=[O:15])[CH3:14])[CH:10]=3)[N:5]=[CH:4][N:3]=2)[CH:26]=[CH:27][CH:28]=1)#[CH:21]

参加物

3

反応物 2

HCID 104682Benzenamine, 3-ethynyl-HCID 272813776,7-Diacetoxy-4-chloro-quinazoline

生成物 1

HCID 16733971HCID 16733971、化合物収率 79%

反応条件

温度
27.5 °C

実験手順

Into a 2.0 Lt four-necked round-bottomed flask, equipped with a mechanical stirrer, reflux condenser and thermometer socket are charged the organic layer from the previous stage (Step 3) containing 4-Chloro-6,7-diacetoxy-quinazoline and 3-ethynylaniline (20 g). The reaction mass was slowly heated to reach reflux condition and maintained and reflux for 14 hours and the reaction was found to be over by HPLC. Then the reaction was cooled to 25-30° C. and filtered the mass washed the cake with chloroform and dried to get 60 g (79% by theory) of N-(3-ethynylphenyl)-6,7-diacetoxy-4-quinazolinamine hydrochloride as yellow solid.

後処理

  1. customInto a 2.0 Lt four-necked round-bottomed flask, equipped with a mechanical stirrer
  2. temperaturereflux condenser
  3. additionthermometer socket are charged the organic layer from the previous stage (Step 3)
  4. temperatureThe reaction mass was slowly heated
  5. temperatureto reach reflux condition
  6. temperaturemaintained
  7. temperaturereflux for 14 hours
  8. filtrationfiltered the mass
  9. washwashed the cake with chloroform
  10. customdried

出典と根拠

ORDレコード
ord-a925205702f2470e9ecdfd9ba66ec60f
出典データセット
uspto-grants-2011_06
特許番号
US07960545B2

反応ノート

読み込み中…