Sodium Chloride → HCID 178505689、化合物

HRID 1419656

反応式

HRID 1419656 の反応式
[K].CCSC(N(CC(C)C)CC(C)C)=O.[O:16]1[C:20]2([CH2:25][CH2:24][CH:23]([CH:26]3[CH2:31][CH2:30][CH:29]([C:32]4[CH:37]=[CH:36][CH:35]=[C:34]([F:38])[CH:33]=4)[CH2:28][CH2:27]3)[CH2:22][CH2:21]2)[O:19][CH2:18][CH2:17]1.[Cl-].[Na+]>CS(C)=O>[O:16]1[C:20]2([CH2:25][CH2:24][CH:23]([C@H:26]3[CH2:31][CH2:30][C@H:29]([C:32]4[CH:37]=[CH:36][CH:35]=[C:34]([F:38])[CH:33]=4)[CH2:28][CH2:27]3)[CH2:22][CH2:21]2)[O:19][CH2:18][CH2:17]1

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 16181ButylateHCID 5462222PotassiumHCID 213085884-(1,4-Dioxaspiro[4,5]dec-8-yl)-1-(3-fluorophenyl)-cyclohexane

生成物 1

HCID 178505689HCID 178505689、化合物収率 97.3%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
100 °C

実験手順

23.7 g of potassium t.-butylate were added to a solution of 125.3 g of 4-(1,4-dioxaspiro[4,5]dec-8-yl)-1-(3-fluorophenyl)-cyclohexane (cis/trans 50/47) in 630 ml of dimethyl sulphoxide, the mixture was stirred at 100° C. for 2 hrs., cooled and poured into 2500 ml of 5 percent sodium chloride solution. The reaction mixture was extracted with methylene chloride, the organic phase was dried over sodium sulfate, filtered and the filtrate was evaporated. Crystallization of the residue from isopropanol gave 121.9 g of trans-4-(1,4-dioxaspiro[4,5]dec-8-yl)-1-(3-fluorophenyl)cyclohexane as colorless crystals (trans content 99.8%).

後処理

  1. temperature, cooled
  2. extractionThe reaction mixture was extracted with methylene chloride
  3. dry with materialthe organic phase was dried over sodium sulfate
  4. filtrationfiltered
  5. customthe filtrate was evaporated
  6. customCrystallization of the residue from isopropanol

出典と根拠

ORDレコード
ord-5ec8769642e9475c888caa24dee08499
出典データセット
uspto-grants-1999_03
特許番号
US05888423

関連ノート

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