Sodium Sulfite → 3-Hydroxymethyl-4-(methylsulfonyl)nitrobenzene

HRID 396812

反応式

HRID 396812 の反応式
[OH:1][CH2:2][C:3]1[CH:4]=[C:5]([N+:11]([O-:13])=[O:12])[CH:6]=[CH:7][C:8]=1SC.[CH:14]1C=C(Cl)C=C(C(OO)=O)C=1.[O-:25][S:26]([O-:28])=O.[Na+].[Na+]>C(Cl)Cl.CO>[OH:1][CH2:2][C:3]1[CH:4]=[C:5]([N+:11]([O-:13])=[O:12])[CH:6]=[CH:7][C:8]=1[S:26]([CH3:14])(=[O:28])=[O:25]

参加物

6

反応物 3

HCID 24437Sodium SulfiteHCID 70297m-Chloroperbenzoic acidHCID 223168073-Hydroxymethyl-4-(methylthio)nitrobenzene

生成物 1

HCID 223169553-Hydroxymethyl-4-(methylsulfonyl)nitrobenzene収率 67.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3-hydroxymethyl-4-(methylthio)nitrobenzene from step 1 (20 g, 0.10 mol) in CH2Cl2 (500 mL) and MeOH (100 mL), m-CPBA (74 g, 0.30 mol) was added portionwise at 0° C., and the mixture was stirrred for 16 h at room temperature. The mixture was added aqueous Na2SO3 (20 g in 200 mL of water) at 0° C. Organic layer was separated and washed with saturated aqueous NaHCO3 (300 mL), dried over MgSO4, and concentarted in vacuo gave the title compound (15.6 g, 65%).

後処理

  1. customOrganic layer was separated
  2. washwashed with saturated aqueous NaHCO3 (300 mL)
  3. dry with materialdried over MgSO4

出典と根拠

ORDレコード
ord-140c39121b1f478c9525ee309be3571e
出典データセット
uspto-grants-2003_08
特許番号
US06608095B2

関連ノート

読み込み中…