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Ethanol → HCID 178479647, 화합물

HRID 2296349
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HRID 2296349 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][NH2:6].[ClH:7].C(=N)(OCC)[CH:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)O.[CH2:21]([OH:23])C>>[ClH:7].[OH:23][C:21]1[N:1]([CH2:9][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:2][CH2:3][CH2:4][CH2:5][N:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 702EthanolHCID 1045PutrescineHCID 12387918Ethyl 1-hydroxy-1-phenylmethanecarboximidate hydrochloride

생성물 1

HCID 178479647HCID 178479647, 화합물수율 34%

실험 절차

To 200 ml of absolute ethanol was added 1,4-diaminobutane at 0° C. with continuous stirring. To this solution waas added an equal molar amount of ethyl mandelimidate hydrochloride. After stirring at 0°-5° C. for two hours, the suspension was heated under reflux 12 hours then cooled and concentrated to remove any traces of NH3. The concentrated solution was acidified by dropwise addition of ethanolic HCl into the suspension which was then concentrated to dryness and the residue recrystallized several times from CH3CN/ether to yield 14.5 g (34%) of product: mp 179°-181° C. Structure was confirmed by IR and NMR.

후처리

  1. temperaturethe suspension was heated
  2. temperatureunder reflux 12 hours
  3. temperaturethen cooled
  4. concentrationconcentrated
  5. customto remove any traces of NH3
  6. additionThe concentrated solution was acidified by dropwise addition of ethanolic HCl into the suspension which
  7. concentrationwas then concentrated to dryness
  8. customthe residue recrystallized several times from CH3CN/ether

출처 및 근거

ORD 기록
ord-cadabf6a12a44235b18e58b934466783
출처 데이터셋
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04428948

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