Formaldehyde → 5H-Dibenz(b,f)azepine, 10,11-dihydro-2-((4-methyl-1-piperazinyl)methyl)-

HRID 1768655노트

반응식

HRID 1768655 반응식
[CH:1]1[C:11]2[CH2:10][CH2:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[NH:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[CH3:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.[CH2:23]=O>ClC(Cl)C.C(O)(=O)C>[CH3:16][N:17]1[CH2:22][CH2:21][N:20]([CH2:23][C:2]2[CH:3]=[CH:4][C:5]3[NH:6][C:7]4[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=4[CH2:9][CH2:10][C:11]=3[CH:1]=2)[CH2:19][CH2:18]1

참가 물질

6

반응물 3

HCID 712FormaldehydeHCID 10308IminodibenylHCID 531671-Methylpiperazine

생성물 1

HCID 30488975H-Dibenz(b,f)azepine, 10,11-dihydro-2-((4-methyl-1-piperazinyl)methyl)-수율 91%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 63651,1-Dichloroethane용매

실험 절차

10,11-Dihydro-5H-dibenz [b,f]azepine (250 g) was suspended in a mixture of 600 ml of dichloroethane and 600 ml of acetic acid, and 155 ml of 1-methylpiperazine was added dropwise to the suspension. To the mixture was added 42 g of paraformaldehyde at 50° C. followed by stirring for 6 hours. The solvent was distilled off under reduced pressure and the residue was diluted with ethyl acetate. The solution was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to give the product (91%). The obtained product was subjected to the subsequent reaction without particular purification.

후처리

  1. additionwas added dropwise to the suspension
  2. distillationThe solvent was distilled off under reduced pressure
  3. additionthe residue was diluted with ethyl acetate
  4. washThe solution was washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-cf011155c84141b59138b5163e9ca8dd
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05378701

반응 노트

불러오는 중…