13-cis-Acitretin → Acitretin

HRID 1247661

반응식

HRID 1247661 반응식
[CH3:1][C:2]1[C:7](/[CH:8]=[CH:9]/[C:10](/[CH3:20])=[CH:11]/[CH:12]=[CH:13]/[C:14](/[CH3:19])=[CH:15]\[C:16]([OH:18])=[O:17])=[C:6]([CH3:21])[C:5]([CH3:22])=[C:4]([O:23][CH3:24])[CH:3]=1>O1CCCC1>[CH3:1][C:2]1[C:7](/[CH:8]=[CH:9]/[C:10](/[CH3:20])=[CH:11]/[CH:12]=[CH:13]/[C:14](/[CH3:19])=[CH:15]/[C:16]([OH:18])=[O:17])=[C:6]([CH3:21])[C:5]([CH3:22])=[C:4]([O:23][CH3:24])[CH:3]=1

참가 물질

3

반응물 1

HCID 643784113-cis-Acitretin

생성물 1

HCID 5284513Acitretin수율 99.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Crude acetretin (10 g) and butylated hydroxyanisole (0.5 g) were dissolved in tetrahydrofuran (350 ml) at room temperature. The resultant solution was filtered and washed with tetrahydrofuran. The combined filtrate was concentrated under vacuum at 30–35° C. Acetone (100 ml) was added to the residue and stirred for 10 minutes at room temperature. The crystalline product so obtained was filtered, washed with acetone and dried at 25–30° C. under vacuum to obtain pure acitretin (8.2 g, assay 99.4% by HPLC).

후처리

  1. filtrationThe resultant solution was filtered
  2. washwashed with tetrahydrofuran
  3. concentrationThe combined filtrate was concentrated under vacuum at 30–35° C
  4. additionAcetone (100 ml) was added to the residue
  5. customThe crystalline product so obtained
  6. filtrationwas filtered
  7. washwashed with acetone
  8. customdried at 25–30° C. under vacuum

출처 및 근거

ORD 기록
ord-d471693cc2d9406e8ddf63604ecb5683
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129365B2

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