Diphosgene → Methyl 6-chloro-3-isocyanato-2-methylbenzoate

HRID 650906노트

반응식

HRID 650906 반응식
[NH2:1][C:2]1[C:3]([CH3:13])=[C:4]([C:9]([Cl:12])=[CH:10][CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].Cl[C:15](OC(Cl)(Cl)Cl)=[O:16]>C1(C)C=CC=CC=1>[Cl:12][C:9]1[C:4]([C:5]([O:7][CH3:8])=[O:6])=[C:3]([CH3:13])[C:2]([N:1]=[C:15]=[O:16])=[CH:11][CH:10]=1

참가 물질

4

반응물 2

HCID 10426DiphosgeneHCID 21710154Methyl 3-amino-6-chloro-2-methylbenzoate

생성물 1

HCID 21710153Methyl 6-chloro-3-isocyanato-2-methylbenzoate수율 100%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 14.7 grams (0.074 mole) of methyl 3-amino-6-chloro-2-methylbenzoate in 1000 mL of toluene was stirred and 14.6 grams (0.074 mole) of trichloromethyl chloroformate was added dropwise thereto. Upon completion of the addition, the reaction mixture was warmed to reflux where it stirred for about 18 hours. After this time the reaction mixture was concentrated under reduced pressure to a residue, which was assumed to be a theoretical yield (16.7 grams) of the subject compound. The subject compound was taken directly to the next reaction in the sequence.

후처리

  1. additionUpon completion of the addition
  2. temperaturethe reaction mixture was warmed
  3. temperatureto reflux where it
  4. concentrationAfter this time the reaction mixture was concentrated under reduced pressure to a residue, which

출처 및 근거

ORD 기록
ord-9d77af4b16114bcc9c5d2af4302d87ab
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06277847B1

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