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

HRID 844600

反応式

HRID 844600 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

HCID 18377608Methyl 3-amino-2-mercaptobenzoate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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))

出典と根拠

ORDレコード
ord-8113f4e5c38e44d1afa6f969d5450162
出典データセット
uspto-grants-2002_04
特許番号
US06380422B1

関連ノート

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