Water → HCID 178481250, 화합물

HRID 236243

반응식

HRID 236243 반응식
[O-]CC.[Na+].[Na].[H][H].[F:8][C:9]([F:20])([F:19])[C:10]1[CH:11]=[C:12]([CH2:16][C:17]#[N:18])[CH:13]=[CH:14][CH:15]=1.[CH3:21][NH:22][CH:23]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:24](OC)=O.[O-]CC.[Na+].C(O)C.[OH2:41]>C(O)C>[CH3:21][N:22]1[C:17]([NH2:18])=[C:16]([C:12]2[CH:13]=[CH:14][CH:15]=[C:10]([C:9]([F:8])([F:19])[F:20])[CH:11]=2)[C:24](=[O:41])[CH:23]1[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

참가 물질

9

반응물 7

HCID 962WaterHCID 75360m-TrifluoromethylphenylacetonitrileHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 13852358Methyl 2-(methylamino)-2-phenylacetateHCID 23706232Ethanol sodium ethoxideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 178481250HCID 178481250, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In this example, sodium ethoxide was prepared by mixing 3.0 g of metallic sodium with 100 ml of absolute ethanol. After the evolution of hydrogen stopped, a mixture containing 16.0 g of (3-trifluoromethylphenyl)-acetonitrile and 17.1 g of methyl methylamino-phenylacetate was added dropwise to the sodium ethoxide-ethanol mixture. The resulting mixture was then refluxed overnight (about 16 hours) and then cooled to room temperature. The mixture was then added to 300 ml of water and extracted with diethyl ether. The ethyl ether extract was filtered to remove precipitate. The filtrate was concentrated by evaporation affording a solid. This solid was then triturated in ethyl ether. The ethyl ether was then removed from the solid. The solid was washed several times with ethyl ether and then dried overnight affording 6.2 g of the title compound.

후처리

  1. temperatureThe resulting mixture was then refluxed overnight (about 16 hours)
  2. extractionextracted with diethyl ether
  3. extractionThe ethyl ether extract
  4. filtrationwas filtered
  5. customto remove precipitate
  6. concentrationThe filtrate was concentrated by evaporation
  7. customaffording a solid
  8. customThis solid was then triturated in ethyl ether
  9. customThe ethyl ether was then removed from the solid
  10. washThe solid was washed several times with ethyl ether
  11. customdried overnight

출처 및 근거

ORD 기록
ord-87c51af8ec874c3ea49862dcb3db61f7
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04643762

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