Phosphorus tribromide → 4-Chloroisatoic anhydride

HRID 569806ノート

反応式

HRID 569806 の反応式
C([O:8][C:9]([NH:11][C:12]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:13]=1[C:14]([OH:16])=[O:15])=O)C1C=CC=CC=1.P(Br)(Br)Br>C(OCC)C>[Cl:21][C:19]1[CH:18]=[CH:17][C:13]2[C:14](=[O:16])[O:15][C:9](=[O:8])[NH:11][C:12]=2[CH:20]=1

参加物

4

反応物 2

HCID 24614Phosphorus tribromideHCID 292998452-{[(Benzyloxy)carbonyl]amino}-4-chlorobenzoic acid

生成物 1

HCID 3291054-Chloroisatoic anhydride収率 91.9%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 2-benzyloxycarbonylamino-4-chlorobenzoic acid (564 g) and phosphorus tribromide (1.5 kg) in diethyl ether (9 l) was refluxed for 40 hours and allowed to stand at room temperature for 5 days. The resulting precipitates were collected by filtration and washed in turn with diethyl ether (5 l) and ethanol (3 l) to give 7-chloro-2H-3,1-benzoxazine-2,4(1H)-dione (335 g).

後処理

  1. temperaturewas refluxed for 40 hours
  2. customThe resulting precipitates
  3. filtrationwere collected by filtration
  4. washwashed in turn with diethyl ether (5 l) and ethanol (3 l)

出典と根拠

ORDレコード
ord-6dc96533fb65485b807fa9372d5d123a
出典データセット
uspto-grants-1988_03
特許番号
US04734419

反応ノート

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