Propargyl bromide → 1-[10,11-Dihydro-3-methoxy-8-methyl-dibenz[b,f]oxepin-10-yl]-4-(2-propynyl)piperazine

HRID 866615ノート

反応式

HRID 866615 の反応式
C(=O)([O-])[O-].[Na+].[Na+].[CH3:7][O:8][C:9]1[CH:10]=[CH:11][C:12]2[CH2:18][CH:17]([N:19]3[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]3)[C:16]3[CH:25]=[C:26]([CH3:29])[CH:27]=[CH:28][C:15]=3[O:14][C:13]=2[CH:30]=1.[CH2:31](Br)[C:32]#[CH:33]>C(O)CCC>[CH3:7][O:8][C:9]1[CH:10]=[CH:11][C:12]2[CH2:18][CH:17]([N:19]3[CH2:24][CH2:23][N:22]([CH2:33][C:32]#[CH:31])[CH2:21][CH2:20]3)[C:16]3[CH:25]=[C:26]([CH3:29])[CH:27]=[CH:28][C:15]=3[O:14][C:13]=2[CH:30]=1

参加物

5

反応物 3

HCID 7842Propargyl bromideHCID 10340Sodium CarbonateHCID 227679281-[10,11-Dihydro-3-methoxy-8-methyl-dibenz[b,f]oxepin-10-yl]-piperazine

生成物 1

HCID 227678361-[10,11-Dihydro-3-methoxy-8-methyl-dibenz[b,f]oxepin-10-yl]-4-(2-propynyl)piperazine

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒2 回

実験手順

3.8 G. of sodium carbonate are added to a solution of 10 g. of 1-[10,11-dihydro-3-methoxy-8-methyl-dibenz[b,f]oxepin-10-yl]-piperazine in 55 ml. of butanol and then a solution of 2.5 ml. of propargyl bromide in 20 ml. of butanol is added dropwise. Then, the mixture is stirred for 20 hours at room temperature and the solvent is removed by distillation under reduced pressure. After working-up in an analogous manner to that described in Example 13, there is isolated crude 1-[10,11-dihydro-3-methoxy-8-methyl-dibenz[b,f]oxepin-10-yl]-4-(2-propynyl)piperazine in the form of an oil. The dihydrochloride, prepared in ethanol and recrystallized from methanol/ether, melts at 210°-212° C. (with decomposition).

後処理

  1. customthe solvent is removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-b40ac20b22c0459898991ba7a4e26491
出典データセット
uspto-grants-1978_07
特許番号
US04100173

反応ノート

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