Diethyl Ether → 8-Chloro-10,11-dihydro-2-methoxy-11-(4-pyridyl)-dibenz[b,f][1,4]oxazepine

HRID 27625노트

반응식

HRID 27625 반응식
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[O:6][C:7]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][C:8]=3[C:9]([C:11]3[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=3)=[N:10][C:4]=2[CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].CCOCC>O>[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[O:6][C:7]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][C:8]=3[CH:9]([C:11]3[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=3)[NH:10][C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 21226445Aluminium lithium hydride2회HCID 233426618-Chloro-2-methoxy-11-(4-pyridyl)-dibenz[b,f][1,4]oxazepine

생성물 1

HCID 233426508-Chloro-10,11-dihydro-2-methoxy-11-(4-pyridyl)-dibenz[b,f][1,4]oxazepine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A 5.0 g. portion of 8-Chloro-2-methoxy-11-(4-pyridyl)-dibenz[b,f][1,4]oxazepine (Example 1) is added to 2.5 g. of lithium aluminum hydride in 200 ml. of ether. The mixture is stirred and heated under reflux for 4 hours. Water is added dropwise to decompose the excess lithium aluminum hydride. The ether is decanted and the residue is extracted with methylene chloride which is then combined with the ether, dried and evaporated. The residue is crystallized from acetone-hexane giving 8-chloro-10,11-dihydro-2-methoxy-11-(4-pyridyl)-dibenz[b,f][1,4]oxazepine, m.p. 186°-188° C.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 4 hours
  3. customThe ether is decanted
  4. extractionthe residue is extracted with methylene chloride which
  5. customdried
  6. customevaporated
  7. customThe residue is crystallized from acetone-hexane

출처 및 근거

ORD 기록
ord-520f3df4738a44f796d71f3412c387ae
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221714

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