Hydrochloric Acid → 8-Chloro-2,3,4,5-tetrahydrobenzo[b][1,4]oxazepine

HRID 220813노트

반응식

HRID 220813 반응식
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]2[N:6](C(C3C=CC=CC=3)=O)[CH2:7][CH2:8][CH2:9][O:10][C:4]=2[CH:3]=1.Cl>O1CCOCC1>[Cl:1][C:2]1[CH:20]=[CH:19][C:5]2[NH:6][CH2:7][CH2:8][CH2:9][O:10][C:4]=2[CH:3]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 57555329(3-Chloro-7,8-dihydro-6H-5-oxa-9-aza-benzocyclohepten-9-yl)-phenyl-methanone

생성물 1

HCID 575553108-Chloro-2,3,4,5-tetrahydrobenzo[b][1,4]oxazepine수율 47%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

(3-Chloro-7,8-dihydro-6H-5-oxa-9-aza-benzocyclohepten-9-yl)-phenyl-methanone from Example E25.2 (783 mg, 2.7 mmol) was dissolved in dioxan (10 ml) and 6M HCl aqueous solution (50 ml) was added. The mixture was heated at reflux for 20 h then concentrated in vacuo and azeotroped with toluene. The residue was dissolved in diethyl ether and water, basified with NaHCO3 and the layers were partitioned. The organic layer was washed with brine, dried and concentrated in vacuo to yield the title compound (280 mg, 47%).

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 20 h
  3. concentrationthen concentrated in vacuo
  4. customazeotroped with toluene
  5. dissolutionThe residue was dissolved in diethyl ether
  6. customthe layers were partitioned
  7. washThe organic layer was washed with brine
  8. customdried
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e13aa5bebcd242078da81bccf431b438
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202858B2

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