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

HRID 257134

반응식

HRID 257134 반응식
[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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 867Malonic Acid2회HCID 14835681Benzo[d][1,2,3]thiadiazole-7-carbaldehyde

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b1ebc41eaa4d407686e5e1dfc993efc4
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05260423

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