Diphosgene → 5-Chloro-3-methyl isatoic anhydride

HRID 516528ノート

反応式

HRID 516528 の反応式
[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

参加物

4

反応物 2

HCID 10426DiphosgeneHCID 116440442-Amino-5-chloro-3-methylbenzoic acid2 回

生成物 1

HCID 115502595-Chloro-3-methyl isatoic anhydride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
42 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-51852a3c860c4c90b30fec60ec84575f
出典データセット
uspto-grants-2015_08
特許番号
US09113630B2

反応ノート

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