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

HRID 623200ノート

反応式

HRID 623200 の反応式
[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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8025Ethyl formateHCID 21290601HCID 21290601、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-f52bc11aee924cf69a8e0c1482ffef4d
出典データセット
uspto-grants-1988_09
特許番号
US04774248

反応ノート

読み込み中…