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3-Pyridinecarboxaldehyde → 3-[5-(4-Chlorophenyl)-2,3-dihydro-1,3,4-thiadiazol-2-yl]pyridine

HRID 255892
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HRID 255892 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([NH:8][NH2:9])=[S:7])=[CH:4][CH:3]=1.[N:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH:18]=O)[CH:13]=1>C(O)C>[Cl:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]2[S:7][CH:18]([C:14]3[CH:13]=[N:12][CH:17]=[CH:16][CH:15]=3)[NH:9][N:8]=2)=[CH:4][CH:3]=1
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참가 물질

4

반응물 2

HCID 103713-PyridinecarboxaldehydeHCID 124770754-Chloro-thiobenzoic acid hydrazide

생성물 1

HCID 157083633-[5-(4-Chlorophenyl)-2,3-dihydro-1,3,4-thiadiazol-2-yl]pyridine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

39.2 g of p-chlorothiobenzoic acid hydrazide are dissolved in 350 ml of ethanol. Under nitrogen, 21.4 g of pyridine-3-aldehyde (dissolved in 20 ml of ethanol) are added dropwise to this solution. The reaction temperature is kept at 20° C. by cooling. When the addition is complete, the reaction mixture is stirred for 1 hour at reflux temperature and subsequently filtered through finely particulate diatomaceous earth. The filtrate is concentrated to three quarters of its initial volume and the precipitated product is isolated by filtration, washed with hexane and dried, affording the title compound of the formula ##STR8## with a melting point of 106°-108° C. (compound 1.1).

후처리

  1. customis kept at 20° C.
  2. temperatureby cooling
  3. additionWhen the addition
  4. temperatureat reflux temperature
  5. filtrationsubsequently filtered through finely particulate diatomaceous earth
  6. concentrationThe filtrate is concentrated to three quarters of its initial volume
  7. customthe precipitated product is isolated by filtration
  8. washwashed with hexane
  9. customdried

출처 및 근거

ORD 기록
ord-1be53cd740d54dbea094fc9e3c17a57f
출처 데이터셋
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04699913

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