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

HRID 27625ノート

反応式

HRID 27625 の反応式
[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

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 21226445Aluminium lithium hydride2 回HCID 233426618-Chloro-2-methoxy-11-(4-pyridyl)-dibenz[b,f][1,4]oxazepine

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-520f3df4738a44f796d71f3412c387ae
出典データセット
uspto-grants-1980_09
特許番号
US04221714

反応ノート

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