Hydrochloric Acid → 5-Pyrimidinol, 1,4,5,6-tetrahydro-5-phenyl-, monohydrochloride

HRID 623200노트

반응식

HRID 623200 반응식
[ClH:1].Cl.[NH2:3][CH2:4][C:5]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([OH:8])[CH2:6][NH2:7].[CH:15](OCC)=O.O.Cl>C(O)C.CO>[ClH:1].[OH:8][C:5]1([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:4][NH:3][CH:15]=[N:7][CH2:6]1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8025Ethyl formateHCID 21290601HCID 21290601, 화합물

생성물 1

HCID 30874735-Pyrimidinol, 1,4,5,6-tetrahydro-5-phenyl-, monohydrochloride수율 84%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol용매

반응 조건

온도
100 °C

실험 절차

A mixture consisting of 5.56 g (0.0335 mol) of 1,3-diamino-2-phenylpropan-2-ol dihydrochloride (m.p. (inst.)=242° C.) and 2.479 g (0.0335 mol; 2.7 ml) of ethyl formate is heated at 100° C. for 3 h. It is then heated at 100° C. under reduced pressure (vacuum obtained by means of a water-jet pump) for 1 h. The reaction medium is cooled, taken up with CH3OH, acidified with ethanol containing HCl and evaporated to dryness, and the evaporation residue is triturated with ether, acetone and chloroform. The precipitate formed is collected by filtration and then recrystallized from an ethanol/diethyl ether mixture (1:1 v/v) to give 6 g (yield: 84%) of CRL 41 382. M.p. (inst.)=206° C.

후처리

  1. temperatureIt is then heated at 100° C. under reduced pressure (vacuum
  2. temperatureThe reaction medium is cooled
  3. customevaporated to dryness
  4. customthe evaporation residue is triturated with ether, acetone and chloroform
  5. customThe precipitate formed
  6. filtrationis collected by filtration
  7. customrecrystallized from an ethanol/diethyl ether mixture (1:1 v/v)
  8. customto give 6 g (yield: 84%) of CRL 41 382
  9. customM.p. (inst.)=206° C.

출처 및 근거

ORD 기록
ord-f52bc11aee924cf69a8e0c1482ffef4d
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04774248

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