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

HRID 2260662ノート

反応式

HRID 2260662 の反応式
[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

参加物

6

反応物 3

HCID 712FormaldehydeHCID 10308IminodibenylHCID 531671-Methylpiperazine

生成物 1

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

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 63651,1-Dichloroethane溶媒

実験手順

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.

後処理

  1. additionwas added dropwise to the suspension To the mixture
  2. distillationwas 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

出典と根拠

ORDレコード
ord-ad94f504a30e44d0950612c65a0cb47d
出典データセット
uspto-grants-1995_12
特許番号
US05478840

反応ノート

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