Phosgene → 6,7-Difluoroisatoic anhydride

HRID 542813ノート

反応式

HRID 542813 の反応式
[C:1](Cl)(Cl)=[O:2].[NH2:5][C:6]1[CH:14]=[C:13]([F:15])[C:12]([F:16])=[CH:11][C:7]=1[C:8]([OH:10])=[O:9]>C1(C)C=CC=CC=1.C(=O)([O-])[O-].[Na+].[Na+]>[F:16][C:12]1[C:13]([F:15])=[CH:14][C:6]2[NH:5][C:1](=[O:2])[O:9][C:8](=[O:10])[C:7]=2[CH:11]=1

参加物

5

反応物 2

HCID 6371PhosgeneHCID 7359652-Amino-4,5-difluorobenzoic acid

生成物 1

HCID 109324446,7-Difluoroisatoic anhydride

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 10340Sodium Carbonate溶媒

実験手順

A solution of phosgene (45 g) in toluene (160 ml) was added during 20 minutes to a stirred solution of 2-amino-4,5-difluorobenzoic acid (26 g) in aqueous sodium carbonate (20.7 g anhydrous sodium carbonate in 350 ml water), keeping the temperature below 40°. The mixture was stirred at room temperature for 15 hours. The solid product was collected by filtration, washed with water and dried to give the novel compound 6,7-difluoro-1H-3,1-benzoxazine-2,4-dione, m.p. 223°-226° (dec.).

後処理

  1. customthe temperature below 40°
  2. filtrationThe solid product was collected by filtration
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-ee7484dae505460e88354dcb0036fcd6
出典データセット
uspto-grants-1987_04
特許番号
US04659718

反応ノート

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