Hydrochloric Acid → 1,3,5-Triazin-2-amine, 4-ethoxy-6-(trifluoromethyl)-

HRID 1598947노트

반응식

HRID 1598947 반응식
[C:1]([NH:3][C:4]([NH2:6])=[NH:5])#[N:2].[F:7][C:8]([F:15])([F:14])[C:9](OCC)=O.[O-:16][CH2:17][CH3:18].[Na+].[Cl-].[Ca+2].[Cl-].Cl>C(O)C>[NH2:5][C:4]1[N:3]=[C:1]([O:16][CH2:17][CH3:18])[N:2]=[C:9]([C:8]([F:7])([F:14])[F:15])[N:6]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 9794Ethyl trifluoroacetateHCID 2723922Sodium ethoxideHCID 5284359Calcium ChlorideHCID 178418324HCID 178418324, 화합물

생성물 1

HCID 1999471,3,5-Triazin-2-amine, 4-ethoxy-6-(trifluoromethyl)-수율 89%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

8.4 g (0.1 mol) of cyanoguanidine and 35.5 g (0.25 mol) of ethyl trifluoroacetate are initially introduced into 46 g of ethanol, and a suspension of 8.5 g (0.125 mol) of sodium ethoxide in 39.8 g of ethanol is added in the course of 5 min. After the addition of 5.66 g (0.05 mol) of calcium chloride, the reaction mixture is heated to reflux for 7 hours. 0.5 ml of a conc. hydrochloric acid is then added at 20° C. and the ethanol is removed. 100 g of water are added and the suspension is filtered with suction. The residue is washed with 50 ml of water and dried at 50° C./20 mbar. 18.6 g (0.089 mol, 89%) of 2-amino-4-ethoxy-6-trifluoromethyl-1,3,5-triazine are obtained in the form of a colorless powder (HPLC: 99.8 area %, m.p. 124°-125° C.).

후처리

  1. additionis added in the course of 5 min
  2. temperaturethe reaction mixture is heated
  3. temperatureto reflux for 7 hours
  4. customthe ethanol is removed
  5. addition100 g of water are added
  6. filtrationthe suspension is filtered with suction
  7. washThe residue is washed with 50 ml of water
  8. customdried at 50° C./20 mbar

출처 및 근거

ORD 기록
ord-332a7fc1d056469db36fcd54e4fb80fa
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05739328

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