Phosphorus tribromide → 4-Chloroisatoic anhydride

HRID 569806노트

반응식

HRID 569806 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 3291054-Chloroisatoic anhydride수율 91.9%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-6dc96533fb65485b807fa9372d5d123a
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04734419

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