2-Chlorotoluene → Mepronil

HRID 487748

반응식

HRID 487748 반응식
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH3:8].[CH:9]([O:12][C:13]1[CH:14]=[C:15]([CH:17]=[CH:18][CH:19]=1)[NH2:16])([CH3:11])[CH3:10].C1(P(C2C=CC=CC=2)CCCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:50](=[O:53])([O-])[O-].[Na+].[Na+].[C]=O>[Pd](Cl)Cl>[CH:9]([O:12][C:13]1[CH:14]=[C:15]([CH:17]=[CH:18][CH:19]=1)[NH:16][C:50]([C:2]1[C:3]([CH3:8])=[CH:4][CH:5]=[CH:6][CH:7]=1)=[O:53])([CH3:11])[CH3:10]

참가 물질

7

반응물 5

HCID 72382-ChlorotolueneHCID 10340Sodium CarbonateHCID 821241,4-Bis(diphenylphosphino)butaneHCID 5732203-IsopropoxyanilineHCID 178418416HCID 178418416, 화합물2회

생성물 1

HCID 41632Mepronil수율 48.7%

시약·촉매·용매 1

HCID 24290Palladium Chloride촉매

실험 절차

In an autoclave made of a metal were placed 12.7 g of ortho-chlorotoluene, 3 g of meta-isopropoxyaniline, 17.7 mg of palladium chloride, 426 mg of 1,4-bisdiphenylphosphinobutane and 23 g of sodium carbonate. The air in the autoclave was replaced with carbon monoxide introduced thereinto in several times, after which carbon monoxide was further introduced to adjust its pressure therein to 30 kg/cm2. The internal temperature was adjusted to 200° C. on a salt bath and the reaction was carried out thereon with stirring for 5 hours. After completion of the reaction, the reaction mixture was cooled to room temperature and washed with water. Subsequently, the organic layer was separated, concentrated, and then recrystallized from ethyl acetatehexane to obtain 2.6 g of 3'-isopropoxy-2-toluanilide.

후처리

  1. additionintroduced
  2. customThe internal temperature was adjusted to 200° C. on a salt bath
  3. customAfter completion of the reaction
  4. washwashed with water
  5. customSubsequently, the organic layer was separated
  6. concentrationconcentrated
  7. customrecrystallized from ethyl acetatehexane

출처 및 근거

ORD 기록
ord-729a6d3dd161469c9dc4a35575be1157
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05296601

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