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

HRID 236521ノート

反応式

HRID 236521 の反応式
[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]

参加物

4

反応物 2

HCID 222AmmoniaHCID 138527082,3-Dichlorobenzenesulfonyl isocyanate

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4e3d0912f6934d6184133f7a64d678af
出典データセット
uspto-grants-1987_02
特許番号
US04645527

反応ノート

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