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Phenyl isocyanate → HCID 135735619, 화합물

HRID 1156754
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HRID 1156754 반응식
[OH:1][CH2:2][C:3]1[CH:15]=[C:14]2[N:5]([C:6](=[O:16])[NH:7][C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=32)[N:4]=1.[C:17]1([N:23]=[C:24]=[O:25])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(OCC)(=O)C>N1C=CC=CC=1>[C:17]1([NH:23][C:24]([O:1][CH2:2][C:3]2[CH:15]=[C:14]3[N:5]([C:6](=[O:16])[NH:7][C:8]4[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=43)[N:4]=2)=[O:25])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7672Phenyl isocyanateHCID 8857Ethyl AcetateHCID 135449340Pirquinozol

생성물 1

HCID 135735619HCID 135735619, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2.0 g (0.0093 mole) of 2-(hydroxymethyl)pyrazolo[1,5-c]-quinazolin-5(6H)-one prepared as described in Example 6B and 1.55 ml (≅1.7 g or 0.014 mole) of 98% phenylisocyanate are refluxed in 20 ml of dry pyridine under N2 for 1 hour. The crude product is poured onto 200 ml of ice-water layered with ethyl acetate (50 ml) and stirred for 30 minutes. The precipitates that form are filtered off, air-dried and taken up in dioxane (150 ml). The solution is filtered while hot and the clear filtrate concentrated down to a volume of 100 ml and cooled. The precipitates are filtered off and dried in vacuo at 85°. Yield 2.45 g, 78.8% crude yield.

후처리

  1. customThe precipitates that form
  2. filtrationare filtered off
  3. customair-dried
  4. filtrationThe solution is filtered while hot and the clear filtrate
  5. concentrationconcentrated down to a volume of 100 ml
  6. temperaturecooled
  7. filtrationThe precipitates are filtered off
  8. customdried in vacuo at 85°

출처 및 근거

ORD 기록
ord-9e9429e2ccbd4158bf6fd858958275e1
출처 데이터셋
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04337255

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