Tetrahydrofuran → HCID 178471528、化合物

HRID 1975616ノート

反応式

HRID 1975616 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][CH2:12][CH:11]([CH:14]=O)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[OH-:16].[K+].[O:18]1[CH2:22][CH2:21][CH2:20][CH2:19]1>O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C@H:8]2[CH2:9][CH2:10][C@H:11](/[CH:14]=[CH:20]/[C:19]([O:18][CH2:22][CH3:21])=[O:16])[CH2:12][CH2:13]2)=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 14797Potassium HydroxideHCID 190979014-(4-Bromophenyl)-cyclohexanecarboxaldehyde

生成物 1

HCID 178471528HCID 178471528、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 9.1 g of 4-(4-bromophenyl)cyclohexanecarb-oxaldehyde and 3.8 g of powdered potassium hydroxide in 200 ml of tetrahydrofuran was placed at room temperature in a sulphonation flask while gassing with argon and treated with 9.2 g of triethyl phosphonoacetate within 15 minutes, stirred overnight, taken up in 100 ml of water and extracted three times with 100 ml of methylene chloride each time. The organic phases were washed twice with 100 ml of water each time, dried over magnesium sulphate and concentrated. Low-pressure chromato-graphy of the residue (12 g) on silica gel with hexane/ethyl acetate (vol. 9:1) gave 11.7 g of ethyl (E)-3-[trans-4-(4-bromo-phenyl)cyclohexyl]acrylate as colourless crystals.

後処理

  1. customwas placed at room temperature in a sulphonation flask
  2. extractionextracted three times with 100 ml of methylene chloride each time
  3. washThe organic phases were washed twice with 100 ml of water each time
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-088a694ada344cf3aeb140b8ff18f938
出典データセット
uspto-grants-1994_02
特許番号
US05288428

反応ノート

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