Propargyl bromide → 2-Propynylpiperazine

HRID 437824노트

반응식

HRID 437824 반응식
C(=O)([O-])[O-].[Na+].[Na+].COC1C=CC2CC([N:19]3[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]3)C3C=C(C)C=CC=3OC=2C=1.[CH2:31](Br)[C:32]#[CH:33]>C(O)CCC>[C:31]([CH:21]1[CH2:20][NH:19][CH2:24][CH2:23][NH:22]1)#[C:32][CH3:33]

참가 물질

5

반응물 3

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

생성물 1

HCID 665838092-Propynylpiperazine

시약·촉매·용매 1

HCID 2631-Butanol용매2회

실험 절차

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-propynylpiperazine in the form of an oil. The dihydrochloride, prepared in ethanol and recrystallized from methanol/ether, melts at 210°-212° C. (with decomposition).

후처리

  1. customthe solvent is removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-66ef0b4ead964a0f92737c82963b791c
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04032525

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