Riluzole → 2-Hydrazinyl-6-(trifluoromethoxy)-1,3-benzothiazole

HRID 865796

반응식

HRID 865796 반응식
[NH2:1][C:2]1[S:3][C:4]2[CH:10]=[C:9]([O:11][C:12]([F:15])([F:14])[F:13])[CH:8]=[CH:7][C:5]=2[N:6]=1.O.[NH2:17]N.Cl.Cl.NN>C(O)CO>[NH:1]([C:2]1[S:3][C:4]2[CH:10]=[C:9]([O:11][C:12]([F:15])([F:13])[F:14])[CH:8]=[CH:7][C:5]=2[N:6]=1)[NH2:17]

참가 물질

5

반응물 3

HCID 5070RiluzoleHCID 17548Hydrazine, dihydrochlorideHCID 24654Hydrazine hydrate (1:1)

생성물 1

HCID 104221582-Hydrazinyl-6-(trifluoromethoxy)-1,3-benzothiazole수율 90.3%

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

반응 조건

온도
140 °C

실험 절차

To a suspension of 93.6 g of 2-amino-6-trifluoromethoxybenzothiazole in 420 cm3 of ethylene glycol under a stream of nitrogen are added 48 g of hydrazine hydrate and 42 g of hydrazine dihydrochloride. The mixture is heated for 2 hours at 140° C. After cooling, the precipitate is filtered off and triturated with a water/diethyl ether mixture (1/1 by volume). 89.9 g of 2-hydrazino-6-trifluoromethoxybenzothiazole are thus obtained, melting at 208° C.

후처리

  1. temperatureAfter cooling
  2. filtrationthe precipitate is filtered off
  3. customtriturated with a water/diethyl ether mixture (1/1 by volume)

출처 및 근거

ORD 기록
ord-45efd324a5be422a87f5ea1d11e02b26
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05567822

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