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

HRID 129039

反応式

HRID 129039 の反応式
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]

参加物

3

反応物 1

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

生成物 1

HCID 101473624-Isopropyl-6-methoxysaccharin収率 91%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-0a8197a401934a08a1fab500f722f634
出典データセット
uspto-grants-1995_11
特許番号
US05466701

関連ノート

読み込み中…