Ammonia → N-(Aminocarbonyl)-2,3-dichlorobenzenesulfonamide

HRID 236521노트

반응식

HRID 236521 반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[S:9]([N:12]=[C:13]=[O:14])(=[O:11])=[O:10].[NH3:15]>O1CCCC1>[NH2:15][C:13]([NH:12][S:9]([C:3]1[CH:4]=[CH:5][CH:6]=[C:7]([Cl:8])[C:2]=1[Cl:1])(=[O:10])=[O:11])=[O:14]

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 138527082,3-Dichlorobenzenesulfonyl isocyanate

생성물 1

HCID 13852713N-(Aminocarbonyl)-2,3-dichlorobenzenesulfonamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 10.0 g of 2,3-dichlorobenzenesulfonyl isocyanate in 200 mL of dry tetrahydrofuran was cooled to 0° C. and treated with 5.0 mL of anhydrous liquid ammonia, added in a dropwise manner at a rate that maintained the temperature between 0° and 10° C. The resultant white mixture was allowed to warm to room temperature and was stirred overnight. The precipitate was collected by filtration, dissolved in 250 mL of water, and acidified with concentrated hydrochloric acid to yield a white solid. Filtration and air drying gave 7.0 g of the title compound, m.p. 197°-200° C.; NMR (DMSO-d6): δ6.0-6.8 (br s, 2H), 7.6 (t, 1H), 7.8-8.1 (m, 2H), 11.1 (br s, 1H); IR (nujol): 1690 cm-1.

후처리

  1. additionadded in a dropwise manner at a rate that
  2. temperaturemaintained the temperature between 0° and 10° C
  3. filtrationThe precipitate was collected by filtration
  4. dissolutiondissolved in 250 mL of water
  5. customto yield a white solid
  6. filtrationFiltration and air
  7. customdrying

출처 및 근거

ORD 기록
ord-4e3d0912f6934d6184133f7a64d678af
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04645527

반응 노트

불러오는 중…