Tributylamine → HCID 178517388, 화합물

HRID 2357872노트

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HRID 2357872 반응식
[NH2:1][C:2]1[N:6]=[CH:5][NH:4][N:3]=1.C([O:9][C:10](=O)[CH:11]([C:17]1[CH:22]=[C:21]([F:23])[CH:20]=[C:19]([F:24])[C:18]=1[F:25])[C:12](OCC)=[O:13])C.C(N(CCCC)CCCC)CCC>[OH-].[Na+]>[OH:9][C:10]1[C:11]([C:17]2[CH:22]=[C:21]([F:23])[CH:20]=[C:19]([F:24])[C:18]=2[F:25])=[C:12]([OH:13])[N:3]2[N:4]=[CH:5][N:6]=[C:2]2[N:1]=1

참가 물질

5

반응물 3

HCID 7622TributylamineHCID 68637486HCID 68637486, 화합물HCID 178418311HCID 178418311, 화합물

생성물 1

HCID 178517388HCID 178517388, 화합물수율 91.5%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

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온도
180 °C

실험 절차

A mixture of 3-amino-1,2,4-triazole (14 g), diethyl(2,3,5-trifluorophenyl)-malonate (0.17 mol, obtained from Ex. 1) and tributylamine (50 ml) was heated at 180° C. for six hours. The reaction mixture was cooled to about 70° C. After addition of aqueous sodium hydroxide (21 g/200 ml H2O) the reaction mixture was stirred for 30 minutes. After separation of the organic phase the aqueous phase was extracted with diethyl ether. The aqueous phase was acidified with concentrated hydrochloric acid. The precipitate was collected by filtration and dried to yield 43 g of the title compound.

후처리

  1. temperatureThe reaction mixture was cooled to about 70° C
  2. customAfter separation of the organic phase the aqueous phase
  3. extractionwas extracted with diethyl ether
  4. filtrationThe precipitate was collected by filtration
  5. customdried

출처 및 근거

ORD 기록
ord-188ccdc085d6488c9d5f450cebfd9730
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07763622B2

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