Hydrochloric Acid → 2-Chloro-1-[4-(trifluoromethyl)-3-pyridinyl]ethanone hydrochloride

HRID 29266

반응식

HRID 29266 반응식
[F:1][C:2]([F:14])([F:13])[C:3]1[C:8]([C:9]([O:11]C)=O)=[CH:7][N:6]=[CH:5][CH:4]=1.[CH2:15]1C(=O)N([Cl:22])C(=O)C1.[ClH:23]>CC(O)=O.CCOCC>[ClH:22].[Cl:23][CH2:15][C:9]([C:8]1[CH:7]=[N:6][CH:5]=[CH:4][C:3]=1[C:2]([F:1])([F:14])[F:13])=[O:11]

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 31398ChlorosuccinimideHCID 2775680Methyl 4-(trifluoromethyl)nicotinate

생성물 1

HCID 218649392-Chloro-1-[4-(trifluoromethyl)-3-pyridinyl]ethanone hydrochloride수율 49%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 3283Diethyl Ether용매

실험 절차

In a 100 mL flask was placed 1.84 g (9.7 mmol, 1 eq) of methyl 4-trifluoromethylnicotinate in 25 mL of 1 M HCl in CH3COOH. To this was then added 1.3 g of NCS (9.7 mmol, 1 eq) and the reaction allowed to stir overnight (18 h). The mixture was then transferred to a 500 mL Erlenmeyer flask and to this was added 300 mL of 2 M HCl in Et2O with stirring. This resulted in a white precipitate which was then filtered to provide 1.2 g (49%) of the desired 2-chloro-1-[4-(trifluoromethyl)-3-pyridinyl]ethanone hydrochloride as a white solid. 1H-NMR (DMSO-d6) δ 9.21 (s, 1H), 9.02 (d, 1H), 7.94 (d, 1H), 5.19 (s, 2H).

후처리

  1. customIn a 100 mL flask was placed
  2. stirringwith stirring
  3. customThis resulted in a white precipitate which
  4. filtrationwas then filtered

출처 및 근거

ORD 기록
ord-bc486d40f494434eb4c1162bfa92226a
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07420066B2

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