Cesium carbonate → HCID 10670907, 화합물

HRID 129056

반응식

HRID 129056 반응식
C(=O)([O-])[O-:2].[Cs+].[Cs+].[C:7]1([C:13]2[C:14](=[O:18])[O:15][CH2:16][CH:17]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.Cl[CH2:20][N:21]1[C:31](=[O:32])[C:30]2[C:25](=[CH:26][C:27]([O:36][CH3:37])=[CH:28][C:29]=2[CH:33]([CH3:35])[CH3:34])[S:22]1(=[O:24])=[O:23]>CO.CN(C)C=O>[O:18]=[C:14]1[C:13]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[C:17]([O:2][CH2:20][N:21]2[C:31](=[O:32])[C:30]3[C:25](=[CH:26][C:27]([O:36][CH3:37])=[CH:28][C:29]=3[CH:33]([CH3:35])[CH3:34])[S:22]2(=[O:24])=[O:23])[CH2:16][O:15]1

참가 물질

6

반응물 3

HCID 10796Cesium carbonateHCID 99951732-(Chloromethyl)-4-isopropyl-6-methoxybenzo[D]isothiazol-3(2H)-one 1,1-dioxideHCID 10986536HCID 10986536, 화합물

생성물 1

HCID 10670907HCID 10670907, 화합물수율 20%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 6228Dimethylformamide용매

실험 절차

Cesium carbonate (0.82 g) was added to a solution of 3-phenyl-2(5H)-furanone (0.88 g) in methanol (15 mL) and the mixture was stirred at room temperature for one hour and stripped of methanol. 2-Chloromethyl-4-isopropyl-6-methoxysaccharin (1.52 g) was added to a solution of the residue in dimethylformamide (15 mL) and the mixture was stirred at room temperature for two days. Silica gel (4.4 g) was added, volatiles were removed under vacuum, and the solid was subjected to flash chromatography on silica gel using ethyl acetate-hexane (3:7) as eluant. Recrystallization of the product from ethanol-ether gave 2-(2,5-dihydro-2-oxo-3-phenylfuran-4-yl)oxymethyl-4-isopropyl-6-methoxysaccharin as a colorless solid (0.45 g, 20% yield, m.r. 180°-182° C. ).

후처리

  1. stirringthe mixture was stirred at room temperature for two days
  2. additionSilica gel (4.4 g) was added
  3. customvolatiles were removed under vacuum
  4. customRecrystallization of the product from ethanol-ether

출처 및 근거

ORD 기록
ord-1d56cfefff0e479598e4c94eaf10493d
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05466701

연결된 노트

불러오는 중…