Potassium Iodide → 4-[4-[4-(Hydroxydiphenylmethyl)-1-piperidinyl]-1-oxobutyl]-2,2-dimethylphenethyl acetate

HRID 53339

反応式

HRID 53339 の反応式
[C:1]([O:4][CH2:5][CH2:6][CH:7]1[CH:12]=[CH:11][C:10]([C:13](=[O:18])[CH2:14][CH2:15][CH2:16]Cl)=[CH:9][C:8]1([CH3:20])[CH3:19])(=[O:3])[CH3:2].[C:21]1([C:27]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)([CH:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)[OH:28])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(=O)([O-])O.[K+].[I-].[K+]>O.C1(C)C=CC=CC=1>[C:1]([O:4][CH2:5][CH2:6][CH:7]1[CH:12]=[CH:11][C:10]([C:13](=[O:18])[CH2:14][CH2:15][CH2:16][N:32]2[CH2:33][CH2:34][CH:29]([C:27]([OH:28])([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)[CH2:30][CH2:31]2)=[CH:9][C:8]1([CH3:20])[CH3:19])(=[O:3])[CH3:2]

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 15723AzacyclonolHCID 516893Potassium BicarbonateHCID 229063004-(4-Chloro-1-oxobutyl)-2,2-dimethylphenethyl acetate

生成物 1

HCID 229063064-[4-[4-(Hydroxydiphenylmethyl)-1-piperidinyl]-1-oxobutyl]-2,2-dimethylphenethyl acetate

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 1140Toluene溶媒2 回

実験手順

Mix 4-(4-chloro-1-oxobutyl)-2,2-dimethylphenethyl acetate (99.5 g, 0.335 mol), α,α-diphenyl-4-piperidinemethanol (101.8 g, 0.335 mol), potassium hydrogen carbonate (83.8 g, 0.838 mol), potassium iodide (1.00 g, 0.006 mol), toluene (600 mL) and water (220 mL). Stir at reflux for 72 hours, add toluene (200 mL) and deionized water (100 mL). Filter through filter aid while at 80° C. and separate the organic phase. Dry (MgSO4), filter and purify by chromatography (ethyl acetate) to give 4-[4-[4-(hydroxydiphenylmethyl)-1-piperidinyl]-1-oxobutyl]-2,2-dimethylphenethyl acetate as an oily solid.

後処理

  1. temperatureat reflux for 72 hours
  2. filtrationFilter
  3. filtrationthrough filter aid while at 80° C.
  4. customseparate the organic phase
  5. dry with materialDry (MgSO4)
  6. filtrationfilter
  7. custompurify by chromatography (ethyl acetate)

出典と根拠

ORDレコード
ord-1385067a1d49477dbeddb28bd37bd339
出典データセット
uspto-grants-1997_04
特許番号
US05618940

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