Pyridine → 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)-1-buten-2-yl chloroformate

HRID 1163857

반응식

HRID 1163857 반응식
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][CH:7]([N:14]2[CH:18]=[N:17][CH:16]=[N:15]2)[C:8](=[O:13])[C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:4][CH:3]=1.[C:21](Cl)([Cl:23])=[O:22].N1C=CC=CC=1>C1COCC1>[Cl:23][C:21]([O:13][C:8]([C:9]([CH3:11])([CH3:12])[CH3:10])=[C:7]([O:6][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:20][CH:19]=1)[N:14]1[CH:18]=[N:17][CH:16]=[N:15]1)=[O:22]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 6371PhosgeneHCID 39385Triadimefon

생성물 1

HCID 541583091-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)-1-buten-2-yl chloroformate수율 36%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 29.4 g (0.01 mole) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)-2-butanone in 250 ml of THF was added 20 ml of liquid phosgene, followed by 9 ml of pyridine. After 3 days, the mixture was filtered and the filtrate evaporated in vacuum to a residual oil. The oil was dissolved in hot 1-chlorobutane and the solution filtered to remove a little white solid. The filtrate was cooled, precipitating a white solid. The solid was isolated by filtration, providing 12.9 g (36% of theoretical) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)-1-buten-2-yl chloroformate, m.p. 159°-161°. The infrared spectrum showed absorption at ca 1800 cm-1.

후처리

  1. filtrationthe mixture was filtered
  2. customthe filtrate evaporated in vacuum to a residual oil
  3. dissolutionThe oil was dissolved in hot 1-chlorobutane
  4. filtrationthe solution filtered
  5. customto remove a little white solid
  6. temperatureThe filtrate was cooled
  7. customprecipitating a white solid
  8. customThe solid was isolated by filtration

출처 및 근거

ORD 기록
ord-a837e94e05be492685eaca8a382b0e47
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04367089

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