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

HRID 650906ノート

反応式

HRID 650906 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 21710153Methyl 6-chloro-3-isocyanato-2-methylbenzoate収率 100%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9d77af4b16114bcc9c5d2af4302d87ab
出典データセット
uspto-grants-2001_08
特許番号
US06277847B1

反応ノート

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