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

HRID 1165824노트

반응식

HRID 1165824 반응식
[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]

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d5d734cb3f184aa8ade4d56c10f58dd2
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04912108

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