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Hydrochloric Acid → HCID 20380005、化合物

HRID 1448493
ノート
印刷プレビュー

反応式

HRID 1448493 の反応式
[ClH:1].[F:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=[O:33])[CH2:10][CH2:11][CH2:12][N:13]2[CH2:18][CH2:17][CH:16]([C:19](O)([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH2:15][CH2:14]2)=[CH:5][CH:4]=1.Cl>C(O)(C)C>[ClH:1].[C:26]1([C:19]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[C:16]2[CH2:15][CH2:14][N:13]([CH2:12][CH2:11][CH2:10][C:9]([C:6]3[CH:5]=[CH:4][C:3]([F:2])=[CH:8][CH:7]=3)=[O:33])[CH2:18][CH2:17]2)[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 2061821-Butanone, 1-(4-fluorophenyl)-4-(4-(hydroxydiphenylmethyl)-1-piperidinyl)-, hydrochloride

生成物 1

HCID 20380005HCID 20380005、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 17.7 g (0.038 mole) of 4'-fluoro-4-[4-(α-hydroxy-α-phenylbenzyl)piperidino]butyrophenone hydrochloride, 200 ml of 37% HCl, and 200 ml of isopropyl alcohol was heated on a steam bath for 4 hours. The solvent and excess acid were removed at reduced pressure. The remaining residue was treated with benzene and ethanol and heated to remove excess acid. The excess benzene and ethanol were removed, and the residue was dissolved in hot butanone to which ether was added. Upon cooling a solid formed which was recrystallized from ethyl acetate to give the desired product M.P. 190°-191° C.

後処理

  1. temperaturewas heated on a steam bath for 4 hours
  2. customThe solvent and excess acid were removed at reduced pressure
  3. additionThe remaining residue was treated with benzene and ethanol
  4. temperatureheated
  5. customto remove excess acid
  6. customThe excess benzene and ethanol were removed
  7. dissolutionthe residue was dissolved in hot butanone to which ether
  8. additionwas added
  9. temperatureUpon cooling a solid
  10. customformed which
  11. customwas recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-ab0f4d03dac6405881d937e0c05b6846
出典データセット
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04180583

反応ノート

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