Piperazine → 11-(Piperazin-1-yl)dibenzo(b,f)(1,4)oxazepine

HRID 1450186ノート

反応式

HRID 1450186 の反応式
[CH:1]1[C:6]2[C:7](=O)[NH:8][C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[O:11][C:5]=2[CH:4]=[CH:3][CH:2]=1.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.[OH-].[NH4+]>C1(C)C=CC=CC=1.Cl[Ti](Cl)(Cl)Cl>[N:17]1([C:7]2[C:6]3[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=3[O:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]=2)[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1

参加物

6

反応物 3

HCID 4837PiperazineHCID 14923Ammonium HydroxideHCID 72374O-(o-Aminophenoxy)benzoic acid lactam

生成物 1

HCID 706187411-(Piperazin-1-yl)dibenzo(b,f)(1,4)oxazepine

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 1140Toluene溶媒

実験手順

To a stirred solution of 10, 11-dihydro-dibenz[b,f][1,4]oxazepin-11-one in dry toluene at room temperature was added piperazine (Aldrich) followed by the dropwise addition of TiCl4. The reaction mixture was refluxed for 2 hours, cooled to room temperature and then poured into an ammonium hydroxide solution. The resulting mixture was extracted with dichloromethane, and the combined organic phases were then dried (K2CO3) and concentrated. Purification of the product was conducted on silica gel using ethyl acetate:hexane (5:1→4:1) as the eluant to give the title compound.

後処理

  1. temperatureThe reaction mixture was refluxed for 2 hours
  2. extractionThe resulting mixture was extracted with dichloromethane
  3. dry with materialthe combined organic phases were then dried (K2CO3)
  4. concentrationconcentrated
  5. customPurification of the product

出典と根拠

ORDレコード
ord-e2c16a857f2e4b02a37fd904c63a0bdd
出典データセット
uspto-grants-1997_02
特許番号
US05602121

反応ノート

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