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Hydrochloric Acid → 3-(2-Hydroxyethyl)-1-(4-piperidyl)-imidazolidin-2-one

HRID 444454
ノート
印刷プレビュー

反応式

HRID 444454 の反応式
C([N:11]1[CH2:16][CH2:15][CH:14]([N:17]2[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][O:24]C3CCCCO3)[C:18]2=[O:31])[CH2:13][CH2:12]1)(OCC1C=CC=CC=1)=O.Cl.[H][H]>CO.[Pd]>[OH:24][CH2:23][CH2:22][N:19]1[CH2:20][CH2:21][N:17]([CH:14]2[CH2:13][CH2:12][NH:11][CH2:16][CH2:15]2)[C:18]1=[O:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 23463795HCID 23463795、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 234638053-(2-Hydroxyethyl)-1-(4-piperidyl)-imidazolidin-2-one

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of 59.7 g of 1-(1-carbobenzoxy-4-piperidyl)-3-[2(2-tetrahydropyranyloxy)-ethyl]-imidazolidin-2-one in 1,200 ml of absolute methanol is hydrogenated at room temperature and normal pressure with the addition of 1 mol equivalent of hydrochloric acid and 6 g of palladium-on-charcoal catalyst until 2 mol equivalents of hydrogen have been taken up. The catalyst is then filtered off and the filtrate is evaporated under reduced pressure. The residue is freed from moisture which is still adhering, by treatment with toluene. The reaction product is chromatographed on 2 kg of basic aluminium oxide using a mixture of chloroform/methanol (85:15) as the eluant mixture. In this way, 3-(2-hydroxyethyl)-1-(4-piperidyl)-imidazolidin-2-one is obtained in the form of a viscous oil, which is further used without additional purification.

後処理

  1. customis hydrogenated at room temperature
  2. filtrationThe catalyst is then filtered off
  3. customthe filtrate is evaporated under reduced pressure
  4. customThe reaction product is chromatographed on 2 kg of basic aluminium oxide using
  5. additiona mixture of chloroform/methanol (85:15) as the eluant mixture

出典と根拠

ORDレコード
ord-0ba2179fe9da450dbbba9609f375eac2
出典データセット
uspto-grants-1981_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04264599

反応ノート

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