Sulfuric Acid → 5-Nitro-1,3-benzothiazol-2-amine

HRID 1383059노트

반응식

HRID 1383059 반응식
Cl[C:2]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:3]=1[NH2:4].O.O.O.[S-2].[Na+].[Na+].S(=O)(=O)(O)O.[NH2:23][C:24](N)=[S:25].NC1C=C([N+]([O-])=O)C=CC=1S>CCCCOCCO.CO.O>[NH2:23][C:24]1[S:25][C:2]2[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:3]=2[N:4]=1

참가 물질

9

반응물 5

HCID 1118Sulfuric AcidHCID 226912-Chloro-5-nitroanilineHCID 2723790ThioureaHCID 63364002-Amino-4-nitrobenzenethiolHCID 24846073Sodium sulphide trihydrate

생성물 1

HCID 27547595-Nitro-1,3-benzothiazol-2-amine

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 81332-Butoxyethanol용매

반응 조건

온도
120 °C

실험 절차

A solution of 8.63 g of 2-chloro-5-nitroaniline and 9.9 g of sodium sulphide trihydrate in 80 ml of butyl glycol was stirred at 80° C. for 30 minutes. After adding 4.16 ml of concentrated sulphuric acid, 7.6 g of thiourea were added to the 2-amino-4-nitrothiophenol, and the mixture was stirred at 120° C. for 3 hours. The reaction mixture was discharged into 400 ml of water and 50 ml of methanol, and the solid was filtered off with suction and washed with water. 5.4 g of crude 2-amino-5-nitrobenzothiazole, the identity of which was confirmed by TLC comparison with authentic material, were obtained.

후처리

  1. filtrationthe solid was filtered off with suction
  2. washwashed with water
  3. customwere obtained

출처 및 근거

ORD 기록
ord-a2191bc50d554de38efb714c914150a2
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04808723

반응 노트

불러오는 중…