1-Methylpiperazine → HCID 22767842、化合物

HRID 372450ノート

反応式

HRID 372450 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 22767842HCID 22767842、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b8e746b684ae4d61aed3c2463f1e1928
出典データセット
uspto-grants-1978_05
特許番号
US04091023

反応ノート

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