Potassium Carbonate → HCID 178447974、化合物

HRID 1249305ノート

反応式

HRID 1249305 の反応式
[CH2:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([CH2:10][CH2:11][C@H:12]2[CH2:17][CH2:16][C@H:15]([CH:18]=O)[CH2:14][CH2:13]2)[CH2:6][CH2:5]1)[CH2:2][CH3:3].[Br-].[C:21]([C:23]1[CH:48]=[CH:47][C:26]([CH2:27][P+](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=[CH:25][CH:24]=1)#[N:22].C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1>[CH2:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([CH2:10][CH2:11][C@H:12]2[CH2:17][CH2:16][C@H:15]([CH:18]=[CH:27][C:26]3[CH:47]=[CH:48][C:23]([C:21]#[N:22])=[CH:24][CH:25]=3)[CH2:14][CH2:13]2)[CH2:6][CH2:5]1)[CH2:2][CH3:3]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 2778276(4-Cyanobenzyl)triphenylphosphonium bromideHCID 178447982HCID 178447982、化合物

生成物 1

HCID 178447974HCID 178447974、化合物収率 77.9%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 5.6 g of trans-4-[2-(trans-4-propylcyclohexyl)ethyl]cyclohexanecarboxaldehyde, 10.6 g of p-cyanobenzyl-triphenylphosphonium bromide and 200 ml of dioxan was treated with 14.5 g of powdered potassium carbonate and the mixture was heated to boiling for 72 hours. After cooling, the mixture was filtered, the filtrate was concentrated and the residue was chromatographed on silica gel with hexane/diethyl ether (vol. 4:1), thereby obtaining 6.0 g of p-[2-[trans-4-[2-(trans-4-propylcyclohexyl)ethyl]cyclohexyl]vinyl]benzonitrile.

後処理

  1. temperaturethe mixture was heated
  2. temperatureAfter cooling
  3. filtrationthe mixture was filtered
  4. concentrationthe filtrate was concentrated
  5. customthe residue was chromatographed on silica gel with hexane/diethyl ether (vol. 4:1)

出典と根拠

ORDレコード
ord-3e1e059c809f4fa0a239625e61415887
出典データセット
uspto-grants-1986_12
特許番号
US04630896

反応ノート

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