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Methanimidic acid, N-cyano-, ethyl ester → N-cyano-N'-[3-[3-(1-piperidinylmethyl)phenoxy]propyl]formamidine hydrochloride

HRID 745852
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HRID 745852 반응식
[N:1]1([CH2:7][C:8]2[CH:9]=[C:10]([CH:16]=[CH:17][CH:18]=2)[O:11][CH2:12][CH2:13][CH2:14][NH2:15])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:19]([N:21]=[CH:22]OCC)#[N:20].[ClH:26].C(O)C>C(O)C.C(OCC)C>[ClH:26].[C:19]([NH:21][CH:22]=[N:15][CH2:14][CH2:13][CH2:12][O:11][C:10]1[CH:16]=[CH:17][CH:18]=[C:8]([CH2:7][N:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)[CH:9]=1)#[N:20]
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참가 물질

6

반응물 3

HCID 9920370Methanimidic acid, N-cyano-, ethyl esterHCID 102205613-(3-(Piperidin-1-ylmethyl)phenoxy)propan-1-amineHCID 21887872Ethanol hydrochloride

생성물 1

HCID 23312557N-cyano-N'-[3-[3-(1-piperidinylmethyl)phenoxy]propyl]formamidine hydrochloride

시약·촉매·용매 2

HCID 702Ethanol용매2회
HCID 3283
Diethyl Ether
용매

실험 절차

To a solution of 2.48 g of 3-[3-(1-piperidinylmethyl)phenoxy]-1-propanamine (prepared according to British Pat. No. 2,023,123 which is hereby incorporated by reference) in 25 ml of absolute ethanol, are added dropwise 0.98 g of ethyl N-cyano-formimidate in 15 ml of ethanol, under stirring and at room temperature. Stirring is maintained for 30 minutes, and then the ethanol is removed by underpressure distillation. An oil residue is formed, which is then dissolved in 250 ml of ethyl ether, after which 0.95 ml of 10N HCl/ethanol are added, yielding 1.4 g of N-cyano-N'-[3-[3-(1-piperidinylmethyl)phenoxy]propyl]formamidine hydrochloride.

후처리

  1. stirringStirring
  2. temperatureis maintained for 30 minutes
  3. customthe ethanol is removed by underpressure distillation
  4. customAn oil residue is formed

출처 및 근거

ORD 기록
ord-f71b7aba58ad41a5b63dce9f712a6e90
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04600780

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