HCID 22901975、化合物 → HCID 22902007、化合物

HRID 1768630ノート

反応式

HRID 1768630 の反応式
[CH3:1][C:2]([NH:5][S:6]([C:9]1[S:17][C:16]2[S:15](=[O:19])(=[O:18])[N:14]([CH2:20][CH2:21][CH2:22][CH2:23][O:24][CH3:25])[CH2:13][CH:12]([OH:26])[C:11]=2[CH:10]=1)(=[O:8])=[O:7])([CH3:4])[CH3:3].CC(C)=O.OS(O)(=O)=O.O=[Cr](=O)=O>CC(C)=O>[CH3:4][C:2]([NH:5][S:6]([C:9]1[S:17][C:16]2[S:15](=[O:19])(=[O:18])[N:14]([CH2:20][CH2:21][CH2:22][CH2:23][O:24][CH3:25])[CH2:13][C:12](=[O:26])[C:11]=2[CH:10]=1)(=[O:8])=[O:7])([CH3:1])[CH3:3]

参加物

4

反応物 2

HCID 22901975HCID 22901975、化合物HCID 131709961Jones' reagent

生成物 1

HCID 22902007HCID 22902007、化合物収率 80.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of the product from Step A (9.5 g, 0.022 mol) in acetone (20 mL) at -10° C. was added freshly prepared Jones reagent (10 mL) and the mixture was stirred at room temperature for 2 hr. The solvent was evaporated and saturated aqueous sodium bicarbonate was added until the pH of the solution was 6. The aqueous mixture was extracted with ethyl acetate (4×50 mL). The combined extracts were washed with brine (2×10 mL), dried (MgSO4) and evaporated to provide a yellow solid (7.5 g, 78%).

後処理

  1. customThe solvent was evaporated
  2. additionsaturated aqueous sodium bicarbonate was added until the pH of the solution
  3. extractionThe aqueous mixture was extracted with ethyl acetate (4×50 mL)
  4. washThe combined extracts were washed with brine (2×10 mL)
  5. dry with materialdried (MgSO4)
  6. customevaporated

出典と根拠

ORDレコード
ord-78d49e99ccf84590b95d52e2851b54cf
出典データセット
uspto-grants-1995_01
特許番号
US05378703

反応ノート

読み込み中…