1-Amino-2-(4-chlorophenylazo)-naphthalene-5-sulfonamide → 1-Naphthalenesulfonamide, 5,6-diamino-

HRID 1165824ノート

反応式

HRID 1165824 の反応式
[NH2:1][C:2]1[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]([S:12]([NH2:15])(=[O:14])=[O:13])[C:6]=2[CH:5]=[CH:4][C:3]=1[N:16]=NC1C=CC(Cl)=CC=1>Cl>[NH2:1][C:2]1[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]([S:12]([NH2:15])(=[O:13])=[O:14])[C:6]=2[CH:5]=[CH:4][C:3]=1[NH2:16]

参加物

3

反応物 1

HCID 46033111-Amino-2-(4-chlorophenylazo)-naphthalene-5-sulfonamide

生成物 1

HCID 51140071-Naphthalenesulfonamide, 5,6-diamino-収率 101.9%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
70 °C

実験手順

To a solution of 18,1 g (SO mmol) stannous chloride dihydrate in 100 ml concentrated hydrochloric acid was added 10,0 g (27,7 mmol) 1-amino-2-(4-chlorophenylazo)-naphthalene-5-sulphonamide. The mixture was stirred at 70° C. for 3 h. After cooling to 25° C., the mixture was poured into 200 ml ice-water. The precipitate was filtered off and washed with 4N hydrochloric acid. The crude product was stirred with ice-water The precipitate was filtered off and washed with ice-water and ethanol to give 6,7 g 1,2-diamino-naphthalene-5-sulphonamide as a hydrochloride salt.

後処理

  1. temperatureAfter cooling to 25° C.
  2. filtrationThe precipitate was filtered off
  3. washwashed with 4N hydrochloric acid
  4. stirringThe crude product was stirred with ice-water The precipitate
  5. filtrationwas filtered off
  6. washwashed with ice-water and ethanol

出典と根拠

ORDレコード
ord-d5d734cb3f184aa8ade4d56c10f58dd2
出典データセット
uspto-grants-1990_03
特許番号
US04912108

反応ノート

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