1-Methylpiperazine → HCID 22767842, 화합물

HRID 437835노트

반응식

HRID 437835 반응식
Cl[CH:2]1[C:8]2[CH:9]=[C:10]([CH3:13])[CH:11]=[CH:12][C:7]=2[O:6][C:5]2[CH:14]=[CH:15][C:16]([CH3:18])=[CH:17][C:4]=2[CH2:3]1.[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>C(Cl)(Cl)Cl>[CH3:18][C:16]1[CH:15]=[CH:14][C:5]2[O:6][C:7]3[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][C:8]=3[CH:2]([N:23]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[CH2:3][C:4]=2[CH:17]=1

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 2276790610-Chloro-10,11-dihydro-2,8-dimethyl-dibenz[b,f]oxepin

생성물 1

HCID 22767842HCID 22767842, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

0.8 G. of 10-chloro-10,11-dihydro-2,8-dimethyl-dibenz[b,f]oxepin and 0.58 g. of 1-methyl-piperazine are dissolved in 4 ml. of chloroform and heated at reflux for 21 hours. Then, the chloroform is evaporated in vacuo. The residue is partitioned between benzene and aqueous sodium carbonate solution. The benzene solution is extracted with dilute hydrochloric acid. The hydrochloric acid extract is made alkaline with sodium carbonate and extracted with benzene. Thereafter, the benzene extract is washed several times with water, dried over sodium sulfate, evaporated in vacuo, and there is obtained 1-[10,11-dihydro-2,8-dimethyl-dibenz[ b,f]oxepin-10-yl] -4-methyl-piperazine, the dihydrochloride of which melts at 197°- 198° C. (with decomposition).

후처리

  1. temperatureat reflux for 21 hours
  2. customThen, the chloroform is evaporated in vacuo
  3. customThe residue is partitioned between benzene and aqueous sodium carbonate solution
  4. extractionThe benzene solution is extracted with dilute hydrochloric acid
  5. extractionThe hydrochloric acid extract
  6. extractionextracted with benzene
  7. extractionThereafter, the benzene extract
  8. washis washed several times with water
  9. dry with materialdried over sodium sulfate
  10. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-b8e6739e87ae4907982fd7fe467eef6c
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04032525

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