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

HRID 1450186노트

반응식

HRID 1450186 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e2c16a857f2e4b02a37fd904c63a0bdd
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05602121

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