Ethyl orthoformate → HCID 178482140, 화합물

HRID 622711

반응식

HRID 622711 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178482140HCID 178482140, 화합물

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid촉매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bf26f55371854a828c4f5bb935c679d5
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04772622

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