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

HRID 1597560

반응식

HRID 1597560 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 223169553-Hydroxymethyl-4-(methylsulfonyl)nitrobenzene수율 67.5%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

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 stirred 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%).

후처리

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

출처 및 근거

ORD 기록
ord-dbc87c166d6c4a9caac3a84cc843fa8d
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06294558B1

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