Ethyl orthoformate → HCID 178482140、化合物

HRID 622711

反応式

HRID 622711 の反応式
[NH:1]([C:5]1[S:6][CH:7]=[C:8]([C:10]2[CH:11]=[C:12]([NH2:16])[CH:13]=[CH:14][CH:15]=2)[N:9]=1)[C:2]([NH2:4])=[NH:3].[CH2:17](OC(OCC)OCC)C>FC(F)(F)C(O)=O>[NH:1]([C:5]1[S:6][CH:7]=[C:8]([C:10]2[CH:11]=[C:12]([NH:16][CH3:17])[CH:13]=[CH:14][CH:15]=2)[N:9]=1)[C:2]([NH2:4])=[NH:3]

参加物

4

反応物 2

HCID 31214Ethyl orthoformateHCID 1785126111-(4-(3-Aminophenyl)thiazol-2-yl)guanidine

生成物 1

HCID 178482140HCID 178482140、化合物

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid触媒

反応条件

温度
0 °C

実験手順

A mixture of 9.3 g (0.04 mole) of 3-(2-guanidino-4-thiazolyl)benzeneamine, 20 ml of triethylorthoformate, and 2 drops of trifluoroacetic acid is stirred at reflux for 5 hours after which it is concentrated in vacuo. The residue is dissolved in 20 ml of ethanol, the solution cooled to 0° C. and then treated with excess sodium borohydride. The mixture is allowed to warm to room temperature, then stirred at reflux for 4 hours. Upon concentration in vacuo the residue is partitioned between water and dichloromethane.

後処理

  1. temperatureat reflux for 5 hours after which it
  2. concentrationis concentrated in vacuo
  3. dissolutionThe residue is dissolved in 20 ml of ethanol
  4. additiontreated with excess sodium borohydride
  5. temperatureto warm to room temperature
  6. stirringstirred
  7. temperatureat reflux for 4 hours
  8. concentrationUpon concentration in vacuo the residue
  9. customis partitioned between water and dichloromethane

出典と根拠

ORDレコード
ord-bf26f55371854a828c4f5bb935c679d5
出典データセット
uspto-grants-1988_09
特許番号
US04772622

関連ノート

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