13-cis-Acitretin → Acitretin

HRID 1247661

反応式

HRID 1247661 の反応式
[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

参加物

3

反応物 1

HCID 643784113-cis-Acitretin

生成物 1

HCID 5284513Acitretin収率 99.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d471693cc2d9406e8ddf63604ecb5683
出典データセット
uspto-grants-2006_10
特許番号
US07129365B2

関連ノート

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