Sodium benzenethiolate → 1-Phenylmercapto-2,5,9-trimethyl-11-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4,6,8,10-undecapentaene

HRID 3898

反応式

HRID 3898 の反応式
C(O[CH2:5][C:6]([CH3:27])=[CH:7][CH:8]=[C:9]([CH3:26])[CH:10]=[CH:11][CH:12]=[C:13]([CH3:25])[CH:14]=[CH:15][C:16]1[C:21]([CH3:23])([CH3:22])[CH2:20][CH2:19][CH2:18][C:17]=1[CH3:24])(=O)C.[S-:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.[Na+]>C1COCC1.CN(P(N(C)C)(N(C)C)=O)C.C(OCC)C>[C:29]1([S:28][CH2:5][C:6]([CH3:27])=[CH:7][CH:8]=[C:9]([CH3:26])[CH:10]=[CH:11][CH:12]=[C:13]([CH3:25])[CH:14]=[CH:15][C:16]2[C:21]([CH3:22])([CH3:23])[CH2:20][CH2:19][CH2:18][C:17]=2[CH3:24])[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1

参加物

6

反応物 2

HCID 4110039Sodium benzenethiolateHCID 544237292,5,9-Trimethyl-11-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4,6,8,10-undecapentaenyl acetate

生成物 1

HCID 536691651-Phenylmercapto-2,5,9-trimethyl-11-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4,6,8,10-undecapentaene

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒HCID 12679Hexamethylphosphoramide溶媒

実験手順

To a solution of 1.85 g (5 mmol) of 2,5,9-trimethyl-11-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4,6,8,10-undecapentaenyl acetate in 25 ml of anhydrous THF and 8 ml of HMPA is added in portions 0.68 g (5.2 mmol) of sodium thiophenoxide. The resulting mixture is stirred at room temperature for 18 hours and then taken up in 250 ml of diethyl ether. The solution is washed with saturated aqueous NH4Cl and water, dried annd evaporated in vacuo to give an oil. Purification on a silica gel dry column gives the desired product.

後処理

  1. washThe solution is washed with saturated aqueous NH4Cl and water
  2. customdried
  3. customannd evaporated in vacuo
  4. customto give an oil
  5. customPurification on a silica gel
  6. customdry column

出典と根拠

ORDレコード
ord-32560364bc2c4583929e9619527c24ce
出典データセット
uspto-grants-1988_02
特許番号
US04722939

関連ノート

読み込み中…