Water → HCID 9932026、化合物

HRID 2292494ノート

反応式

HRID 2292494 の反応式
Cl([O-])=O.[Na+].[F:5][C:6]1[CH:34]=[CH:33][C:9]([C:10]([C@H:12]2[CH2:17][CH2:16][C@H:15]3[C@H:18]4[C@H:28]([CH2:29][CH2:30][C@:13]23[CH3:14])[C@:26]2([CH3:27])[C:21]([CH:22]=[C:23]([CH:31]=[O:32])[CH2:24][CH2:25]2)=[CH:20][CH2:19]4)=[O:11])=[CH:8][CH:7]=1.P([O-])([O-])([O-])=[O:36].[Na+].[Na+].[Na+].O>CC(=CC)C.C1COCC1.C(O)(=O)C.C(O)(C)(C)C>[F:5][C:6]1[CH:7]=[CH:8][C:9]([C:10]([C@H:12]2[CH2:17][CH2:16][C@H:15]3[C@H:18]4[C@H:28]([CH2:29][CH2:30][C@:13]23[CH3:14])[C@:26]2([CH3:27])[C:21]([CH:22]=[C:23]([C:31]([OH:36])=[O:32])[CH2:24][CH2:25]2)=[CH:20][CH2:19]4)=[O:11])=[CH:33][CH:34]=1

参加物

9

反応物 4

HCID 962WaterHCID 24243Trisodium PhosphateHCID 23668197Sodium ChloriteHCID 54571409HCID 54571409、化合物

生成物 1

HCID 9932026HCID 9932026、化合物

試薬・触媒・溶媒 4

HCID 176Acetic Acid溶媒HCID 6386tert-Butanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 105532-Methyl-2-butene溶媒

実験手順

Sodium chlorite is added to a mixture of 17β-(4-fluorobenzoyl)-androsta-3,5-diene-3-carboxaldehyde, sodium phosphate, monobasic monohydrate in 2-methyl-2-butene in THF, H2O, and t-butanol at RT. After 6 h acetic acid was added, then the aqueous layer is extracted with EtOAc, the combined organic extracts are dried (MgSO4), filtered, concentrated, and flash chromatographed to yield the title compound.

後処理

  1. customat RT
  2. extractionthe aqueous layer is extracted with EtOAc
  3. dry with materialthe combined organic extracts are dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customflash chromatographed

出典と根拠

ORDレコード
ord-b2c1cb349a34487c93452157e22a20ca
出典データセット
uspto-grants-1997_11
特許番号
US05683995

反応ノート

読み込み中…