1,2,3-Benzothiadiazole-7-carboxylic acid, methyl ester → Methyl 3-amino-2-mercaptobenzoate

HRID 611783

반응식

HRID 611783 반응식
[S:1]1[C:5]2[C:6]([C:10]([O:12][CH3:13])=[O:11])=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=N1>O1CCOCC1.[Pd]>[NH2:3][C:4]1[C:5]([SH:1])=[C:6]([CH:7]=[CH:8][CH:9]=1)[C:10]([O:12][CH3:13])=[O:11]

참가 물질

4

반응물 1

HCID 1794011,2,3-Benzothiadiazole-7-carboxylic acid, methyl ester

생성물 1

HCID 18377608Methyl 3-amino-2-mercaptobenzoate

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 312751,4-Dioxane용매

실험 절차

A solution of 1 g of methyl benzo-1,2,3-thiadiazole-7-carboxylate in 40 ml of dioxane is hydrogenated over 0.5 g of palladium-on-charcoal (5%) at 160° C. under an initial pressure of 150 bar. After the starting substance has reacted completely, the catalyst is filtered off and rinsed with dioxane, the filtrate is evaporated, avoiding contact with air, and the residue is purified over silica gel (hexane/ethyl acetate (6:4)). The title compound of melting point 174-175° C. is obtained by this procedure.

후처리

  1. customAfter the starting substance has reacted completely
  2. filtrationthe catalyst is filtered off
  3. washrinsed with dioxane
  4. customthe filtrate is evaporated
  5. customthe residue is purified over silica gel (hexane/ethyl acetate (6:4))

출처 및 근거

ORD 기록
ord-3ca0b8119f5344e5a7eb428f042f5e73
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06002013

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