Phenyl isocyanate → Prinomide

HRID 127584

반응식

HRID 127584 반응식
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7](=[O:11])[CH2:8][C:9]#[N:10].[C:12]1([N:18]=[C:19]=[O:20])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C1(C)C=CC=CC=1.C(N(CC)CC)C>[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7](=[O:11])[CH:8]([C:19](=[O:20])[NH:18][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:9]#[N:10]

참가 물질

5

반응물 2

HCID 7672Phenyl isocyanateHCID 27771703-(1-Methyl-1H-pyrrol-2-yl)-3-oxopropanenitrile

생성물 1

HCID 60352Prinomide

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8471Triethylamine용매

실험 절차

To the suspension of 12.9 of 1-methyl-β-oxo-2-pyrrolpropionitrile in 150 ml of dry toluene and 10.1 g of anhydrous triethylamine, 10.7 g of phenylisocyanate are added while stirring. After all solids are dissolved, the dark red solution is allowed to stand 30 minutes at room temperature, 5 minutes on the steam cone and at room temperature overnight. The mixture is evaporated on the steam cone, the residue taken up in methanol and the solution poured into the mixture of 25 ml of 5 N hydrochloric acid and 600 ml of water. The light brown crystals formed are collected, washed with water, triturated with ethanol and recrystallized from about 2200 ml of methanol, to yield the 1-methyl-β-oxo-α-phenylcarbamoyl-2-pyrrol-propionitrile of the formula ##STR8## melting at 174°-175°.

후처리

  1. additionare added
  2. dissolutionAfter all solids are dissolved
  3. customThe mixture is evaporated on the steam cone
  4. additionthe solution poured into the mixture of 25 ml of 5 N hydrochloric acid and 600 ml of water
  5. customThe light brown crystals formed
  6. customare collected
  7. washwashed with water
  8. customtriturated with ethanol
  9. customrecrystallized from about 2200 ml of methanol

출처 및 근거

ORD 기록
ord-238cd5b3ea2c4614a5457f8993b6ac32
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256759

연결된 노트

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