Hydrochloric Acid → 1,2,3-Benzothiadiazole-7-carboxylic acid

HRID 1612635

反応式

HRID 1612635 の反応式
C[O:2][C:3]([C:5]1[C:13]2[S:12][N:11]=[N:10][C:9]=2[CH:8]=[CH:7][CH:6]=1)=[O:4].[OH-].[Na+].O1CCOCC1.Cl>O>[S:12]1[C:13]2[C:5]([C:3]([OH:4])=[O:2])=[CH:6][CH:7]=[CH:8][C:9]=2[N:10]=[N:11]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 312751,4-DioxaneHCID 1794011,2,3-Benzothiadiazole-7-carboxylic acid, methyl ester

生成物 1

HCID 109211091,2,3-Benzothiadiazole-7-carboxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
40 °C

実験手順

100 g (0.51 mol) of 7-methoxycarbonylbenzo-1,2,3-thiadiazole are suspended in 1000 ml of water, and then 310 ml of 2N sodium hydroxide solution and 5 ml of dioxane are added. The reaction mixture is heated to 40° C., is stirred for 4 hours at that temperature and is then cooled to 10° C. A further 1000 ml of water are added and the batch is neutralised with 310 ml of 2N hydrochloric acid. The resulting precipitate is isolated by filtration, lightly dried in a current of air and then dissolved in tetrahydrofuran and the solution is dried over magnesium sulfate, filtered and concentrated. The crystals are suspended in hexane, isolated by filtration and dried.

後処理

  1. temperatureis then cooled to 10° C
  2. customThe resulting precipitate is isolated by filtration
  3. customlightly dried in a current of air
  4. dissolutiondissolved in tetrahydrofuran
  5. dry with materialthe solution is dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customisolated by filtration
  9. customdried

出典と根拠

ORDレコード
ord-5b24337a92d343fbbef2a65fcdae2f8d
出典データセット
uspto-grants-1993_03
特許番号
US05190928

関連ノート

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