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Ammonia → 4-Allylamino-2-amino-6-nitroquinazoline

HRID 1250594
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인쇄 미리보기

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HRID 1250594 반응식
[NH3:1].[CH2:2]([NH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([N+:16]([O-:18])=[O:17])[CH:14]=2)[N:9]=[C:8](Cl)[N:7]=1)[CH:3]=[CH2:4].O>C(O)C.C1COCC1>[CH2:2]([NH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([N+:16]([O-:18])=[O:17])[CH:14]=2)[N:9]=[C:8]([NH2:1])[N:7]=1)[CH:3]=[CH2:4]
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참가 물질

6

반응물 3

HCID 222AmmoniaHCID 962WaterHCID 183264874-Allylamino-2-chloro-6-nitroquinazoline

생성물 1

HCID 183264494-Allylamino-2-amino-6-nitroquinazoline수율 84.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
70 °C

실험 절차

After 10 ml of ammonia gas was dissolved in 50 ml of ethanol at −78° C., 15 ml of a solution of 2.40 g (9.07 mmol) of 4-allylamino-2-chloro-6-nitroquinazoline in THF was added thereto, followed by stirring overnight in a sealed tube at 70° C. 150 ml of water was added to the reaction solution, and then crystals thus precipitated were filtered out, followed by recrystallization from ethyl acetate-hexane to give 1.88 g (84.6%) of the title compound.

후처리

  1. customcrystals thus precipitated
  2. filtrationwere filtered out
  3. customfollowed by recrystallization from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-7c7ed0f66cac43b9ae8d0ea76fa0da79
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06339089B2

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