Triethylamine → HCID 178517389, 화합물

HRID 23906

반응식

HRID 23906 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([F:9])[C:3]=1[CH:10]([C:16]([O:18]CC)=O)[C:11](OCC)=[O:12].C(N(CC)CC)C.[NH2:28][C:29]1[N:33]=[CH:32][NH:31][N:30]=1.[OH-].[Na+]>O>[OH:18][C:16]1[C:10]([C:3]2[C:2]([F:1])=[CH:7][C:6]([F:8])=[CH:5][C:4]=2[F:9])=[C:11]([OH:12])[N:30]2[N:31]=[CH:32][N:33]=[C:29]2[N:28]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 2782662Propanedioic acid, 2-(2,4,6-trifluorophenyl)-, 1,3-diethyl esterHCID 178418311HCID 178418311, 화합물

생성물 1

HCID 178517389HCID 178517389, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
180 °C

실험 절차

A mixture of 22 mmol of diethyl 2-(2,4,6-trifluorophenyl)malonate, 24 mmol of triethylamine and 22 mmol of 3-amino-1,2,4-triazole was heated with stirring at 180° C. for 6 hours. The reaction mixture was then cooled to 50° C., admixed with a solution of 2.2 g of sodium hydroxide in 25 ml of water and stirred for 30 minutes. The aqueous phase was washed with ether and then acidified with conc. hydrochloric acid. The precipitated colorless solid was filtered off, washed with water and diisopropyl ether and dried. The yield of the title compound was 85% (m.p.: 200-201° C.).

후처리

  1. temperaturewas heated
  2. temperatureThe reaction mixture was then cooled to 50° C.
  3. stirringstirred for 30 minutes
  4. washThe aqueous phase was washed with ether
  5. filtrationThe precipitated colorless solid was filtered off
  6. washwashed with water and diisopropyl ether
  7. customdried

출처 및 근거

ORD 기록
ord-44d9929e86744a49a72323548ff6e76e
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06855718B2

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