Triethylamine → N,N-dimethyl-2-(3-trifluoromethylbenzoyl) nicotinamide

HRID 275261노트

반응식

HRID 275261 반응식
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][CH:19]=1)[C:6]([C:8]1[N:16]=[CH:15][CH:14]=[CH:13][C:9]=1[C:10](Cl)=[O:11])=[O:7].Cl.[CH3:23][NH:24][CH3:25].C(N(CC)CC)C>C1(C)C=CC=CC=1.C(OCC)(=O)C>[CH3:23][N:24]([CH3:25])[C:10](=[O:11])[C:9]1[CH:13]=[CH:14][CH:15]=[N:16][C:8]=1[C:6](=[O:7])[C:5]1[CH:17]=[CH:18][CH:19]=[C:3]([C:2]([F:21])([F:20])[F:1])[CH:4]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 200876762-(3-Trifluoromethylbenzoyl)nicotinoyl chloride

생성물 1

HCID 20087671N,N-dimethyl-2-(3-trifluoromethylbenzoyl) nicotinamide

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

The product from step (i) above was dissolved in dry toluene (10 ml). Dimethylamine hydrochloride (1.3 g) was added followed by triethylamine (1.94 g). The mixture was then stirred at room temperature for 4.5 hours. The mixture was diluted with ethyl acetate and washed successively with ethyl acetate and washed successively with 2N sodium carbonate, 2N hydrochloric acid then water. The organic phase was dried then evaporated to yield a red-brown gum which was triturated in hexane to yield the title product as a beige solid (0.64 g), m.p.100°-103° C.

후처리

  1. washwashed successively with ethyl acetate
  2. washwashed successively with 2N sodium carbonate, 2N hydrochloric acid
  3. customThe organic phase was dried
  4. customthen evaporated
  5. customto yield a red-brown gum which
  6. customwas triturated in hexane

출처 및 근거

ORD 기록
ord-71b361b3751340398fd8c6ee48cbe87b
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05393730

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