Diphosgene → 5-Chloro-3-methyl isatoic anhydride

HRID 516528노트

반응식

HRID 516528 반응식
[NH2:1][C:2]1[C:10]([CH3:11])=[CH:9][C:8]([Cl:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Cl[C:14](OC(Cl)(Cl)Cl)=[O:15]>O1CCOCC1>[Cl:12][C:8]1[CH:9]=[C:10]([CH3:11])[C:2]2[NH:1][C:14](=[O:15])[O:5][C:4](=[O:6])[C:3]=2[CH:7]=1

참가 물질

4

반응물 2

HCID 10426DiphosgeneHCID 116440442-Amino-5-chloro-3-methylbenzoic acid2회

생성물 1

HCID 115502595-Chloro-3-methyl isatoic anhydride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
42 °C

실험 절차

To a suspension of 2-amino-3-methyl-5-chlorobenzoic acid (i.e. product of Example 6, Step A) (97 g, 520 mmol) stirred in dry dioxane (750 mL) at room temperature, trichloromethyl chloroformate (63 g, 320 mmol) was added dropwise. The reaction mixture exothermically warmed slowly to 42° C., and the solid almost completely dissolved before a thick suspension formed again. After the suspension was stirred at ambient temperature for 2.5 hours, the title compound was isolated by filtration, washed with ethyl ether, and dried to yield the title product compound, obtained as a white solid (98 g).

후처리

  1. dissolutionthe solid almost completely dissolved before a thick suspension
  2. customformed again

출처 및 근거

ORD 기록
ord-51852a3c860c4c90b30fec60ec84575f
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09113630B2

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