Benzamide, 2-(aminosulfonyl)-N,N-diethyl-4-methoxy-6-(1-methylethyl)- → 4-Isopropyl-6-methoxysaccharin

HRID 129039

반응식

HRID 129039 반응식
N[S:2]([C:5]1[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[C:14]([CH:20]([CH3:22])[CH3:21])[C:6]=1[C:7]([N:9](CC)CC)=[O:8])(=[O:4])=[O:3]>C(O)(=O)C>[CH:20]([C:14]1[CH:15]=[C:16]([O:18][CH3:19])[CH:17]=[C:5]2[C:6]=1[C:7](=[O:8])[NH:9][S:2]2(=[O:4])=[O:3])([CH3:22])[CH3:21]

참가 물질

3

반응물 1

HCID 10336632Benzamide, 2-(aminosulfonyl)-N,N-diethyl-4-methoxy-6-(1-methylethyl)-

생성물 1

HCID 101473624-Isopropyl-6-methoxysaccharin수율 91%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 2.aminosulfonyl-6-isopropyl-4-methoxy-N,N-diethylbenzamide (429.6 g) in acetic acid (1.5 L) was refluxed for 20 hours, then cooled to room temperature. The solvent was removed under vacuum. The oily residue was dissolved in water (6 L) and the pH was adjusted to 1 with hydrochloric acid (6N). The crude product was collected by filtration, washed with water (2 L), dried at 60° C. under vacuum for 18 hours and recrystallized from ethyl acetate-hexane to give 4-isopropyl-6-methoxysaccharin (303 g, 91% yield, m.p. 188° C.).

후처리

  1. customThe solvent was removed under vacuum
  2. dissolutionThe oily residue was dissolved in water (6 L)
  3. filtrationThe crude product was collected by filtration
  4. washwashed with water (2 L)
  5. customdried at 60° C. under vacuum for 18 hours
  6. customrecrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-0a8197a401934a08a1fab500f722f634
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05466701

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