Water → HCID 15428837, 화합물

HRID 1489030노트

반응식

HRID 1489030 반응식
[Cl:1][C:2]1[N:11]=[C:10]([NH:12][NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.C(N(CC)C(C)C)(C)C.[C:29](Cl)(Cl)=[O:30].O>C1COCC1>[Cl:1][C:2]1[N:11]2[C:29](=[O:30])[N:13]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[N:12]=[C:10]2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6371PhosgeneHCID 81531DiisopropylethylamineHCID 154288362-Chloro-4-phenylhydrazinoquinazoline

생성물 1

HCID 15428837HCID 15428837, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of 2-chloro-4-phenylhydrazinoquinazoline (2 g, 7.4 mmol) and N,N-diisopropylethylamine (2 ml, 11.4 mmol) in THF was added phosgene (6 ml, 20% in Toluene) slowly, then stirred for additional 5 min. The reaction mixture was poured into water and extracted with ethyl acetate (2×100 ml). The combined organic layers were washed with brine and dried over Na2SO4 and evaporated under reduced pressure. The residue was triturated with ethanol and filtered to afford 5-chloro-2-phenyl-1,2,4-triazolo[4,3-c]quinazolin-3-one (1.8 g) as a yellow solid. m.p. 167°-168° C.

후처리

  1. extractionextracted with ethyl acetate (2×100 ml)
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over Na2SO4
  4. customevaporated under reduced pressure
  5. customThe residue was triturated with ethanol
  6. filtrationfiltered

출처 및 근거

ORD 기록
ord-ab3233eb6dd74e74b9fe14341621ecb7
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677309

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