Benzenamine, 3-ethynyl- → HCID 16733971, 화합물

HRID 2423006노트

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HRID 2423006 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

HCID 16733971HCID 16733971, 화합물수율 79%

반응 조건

온도
27.5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a925205702f2470e9ecdfd9ba66ec60f
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07960545B2

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