Phosgene → Isopropyl3-(2-chloro-4-fluoro-5-isocyanatophenyl)tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetate

HRID 52417

反応式

HRID 52417 の反応式
[NH2:1][C:2]1[C:3]([F:26])=[CH:4][C:5]([Cl:25])=[C:6]([N:8]2[C:13](=[O:14])[N:12]([CH3:15])[C:11](=[O:16])[N:10]([CH2:17][C:18]([O:20][CH:21]([CH3:23])[CH3:22])=[O:19])[C:9]2=[O:24])[CH:7]=1.[C:27](Cl)(Cl)=[O:28]>C1(C)C=CC=CC=1>[Cl:25][C:5]1[CH:4]=[C:3]([F:26])[C:2]([N:1]=[C:27]=[O:28])=[CH:7][C:6]=1[N:8]1[C:13](=[O:14])[N:12]([CH3:15])[C:11](=[O:16])[N:10]([CH2:17][C:18]([O:20][CH:21]([CH3:23])[CH3:22])=[O:19])[C:9]1=[O:24]

参加物

4

反応物 2

HCID 6371PhosgeneHCID 57313385isopropyl 3-(5-amino-2-chloro-4-fluorophenyl)tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetate

生成物 1

HCID 57228591Isopropyl3-(2-chloro-4-fluoro-5-isocyanatophenyl)tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

A mixture of isopropyl 3-(5-amino-2-chloro-4-fluorophenyl)tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetate (4.0 g, 0.0103 mol) in toluene is treated with a 1.93M solution of phosgene in toluene (19 mL), refluxed for 3 hours, cooled, partially concentrated in vacuo, diluted with toluene, partially concentrated in vacuo, diluted with toluene and concentrated in vacuo to give the title product as a yellow foam which is identified by 1H NMR spectral analysis.

後処理

  1. temperaturerefluxed for 3 hours
  2. temperaturecooled
  3. concentrationpartially concentrated in vacuo
  4. additiondiluted with toluene
  5. concentrationpartially concentrated in vacuo
  6. additiondiluted with toluene
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-815711196f864b7eb0f8224accec6e02
出典データセット
uspto-grants-1997_04
特許番号
US05616706

関連ノート

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