Hydrochloric Acid → 3-[Benzo-1,2,3-thiadiazol-7-yl]acrylic acid

HRID 257134ノート

反応式

HRID 257134 の反応式
[S:1]1[C:5]2[C:6]([CH:10]=O)=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1.C(O)(=O)[CH2:13][C:14]([OH:16])=[O:15].Cl>N1C=CC=CC=1>[S:1]1[C:5]2[C:6]([CH:10]=[CH:13][C:14]([OH:16])=[O:15])=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 867Malonic Acid2 回HCID 14835681Benzo[d][1,2,3]thiadiazole-7-carbaldehyde

生成物 1

HCID 544960903-[Benzo-1,2,3-thiadiazol-7-yl]acrylic acid収率 447.6%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 1.96 g of benzo-1,2,3-thiadiazole-7-carbaldehyde, 1.24 g of malonic acid and 6 ml of pyridine are heated for 26 hours at 120° C., with 2 further additions of 0.6 g portions of malonic acid after 4 and 7 hours. The mixture is then cooled, poured into ice-water and acidified with concentrated hydrochloric acid. The precipitate which has formed is filtered off and dissolved in dilute sodium hydroxide solution, the mixture is washed three times with methylene chloride, and the aqueous phase is subsequently acidified once more, using hydrochloric acid. The precipitate obtained is filtered off, washed with water and dried in vacuo, resulting in 11 g of the title compound of m.p. 199°-202° C.

後処理

  1. temperatureThe mixture is then cooled
  2. customThe precipitate which has formed
  3. filtrationis filtered off
  4. dissolutiondissolved in dilute sodium hydroxide solution
  5. washthe mixture is washed three times with methylene chloride
  6. customThe precipitate obtained
  7. filtrationis filtered off
  8. washwashed with water
  9. customdried in vacuo

出典と根拠

ORDレコード
ord-b1ebc41eaa4d407686e5e1dfc993efc4
出典データセット
uspto-grants-1993_11
特許番号
US05260423

反応ノート

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