Sodium Chloride → HCID 178505689, 화합물

HRID 1419656

반응식

HRID 1419656 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 178505689HCID 178505689, 화합물수율 97.3%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
100 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-5ec8769642e9475c888caa24dee08499
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05888423

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