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

HRID 255892
ノート
印刷プレビュー

反応式

HRID 255892 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 103713-PyridinecarboxaldehydeHCID 124770754-Chloro-thiobenzoic acid hydrazide

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1be53cd740d54dbea094fc9e3c17a57f
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04699913

反応ノート

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