Sodium Acetate → HCID 178481663, 화합물

HRID 839475

반응식

HRID 839475 반응식
[OH-].[CH3:2][N+:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[S:5][C:4]=1SCCCS(O)(=O)=O.Cl.Cl.[NH2:22][C:23]1[CH:31]=[CH:30][C:26]2[NH:27][N:28]=[N:29][C:25]=2[CH:24]=1.C([O-])(=O)C.[Na+]>O>[CH3:2][N:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[S:5](=[N:22][C:23]2[CH:31]=[CH:30][C:26]3[NH:27][N:28]=[N:29][C:25]=3[CH:24]=2)[CH2:4]1

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 867357563-Methyl-2-(3-sulfopropylthio) benzothiazolium hydroxideHCID 178478652HCID 178478652, 화합물

생성물 1

HCID 178481663HCID 178481663, 화합물수율 98.7%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
50 °C

실험 절차

175 g of anhydrous 3-methyl-2-(3-sulfopropylthio) benzothiazolium hydroxide was added to a mixture of 100 g of 5-aminobenzotriazole di-hydrochloride, 120 g of sodium acetate and 1000 ml of water under heating at 50° C with stirring in a 2000 ml flask. After stirring for 1 hour at 85° C the mixture was cooled (15° C) with water. The precipitate formed was collected by filtration, washed with water and then with acetonitrile to yield 135 g of crystals. These crystals were dissolved by heating (90° C) in 350 ml of dimethylformamide and the solution was treated with active carbon and filtered. By addition of 1400 ml of acetonitrile to the filtrate, crystals were formed. The crystals were collected to yield 121 g of the desired compound. The melting point was 240.5° C.

후처리

  1. stirringAfter stirring for 1 hour at 85° C the mixture
  2. customThe precipitate formed
  3. filtrationwas collected by filtration
  4. washwashed with water

출처 및 근거

ORD 기록
ord-83e9387fa1c541aeaaebcb2cb3c4802e
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04095984

연결된 노트

불러오는 중…