Pyridine → HCID 57656832, 화합물

HRID 603170

반응식

HRID 603170 반응식
Cl[C:2]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:3].[Cl:11][C:12]1[CH:13]=[C:14]([CH:16]=[CH:17][C:18]=1[C:19]([F:22])([F:21])[F:20])[NH2:15].N1C=CC=CC=1>C1COCC1.C(OCC)(=O)C.Cl>[Cl:11][C:12]1[CH:13]=[C:14]([NH:15][C:2](=[O:3])[O:4][C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH:16]=[CH:17][C:18]=1[C:19]([F:21])([F:22])[F:20]

참가 물질

7

반응물 3

HCID 1049PyridineHCID 15891Phenyl chloroformateHCID 679623-Chloro-4-(trifluoromethyl)aniline

생성물 1

HCID 57656832HCID 57656832, 화합물

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

Phenyl chloroformate (0.86 mL) was added slowly to a stirring solution of 3-chloro-4-trifluoromethyl aniline (933 mg) in THF (10 mL) containing pyridine (1.07 mL) under an argon atmosphere. The reaction was stirred for 18 h then diluted with ethyl acetate (35 mL) and 1M HCl (20 mL). The organic layer was separated and washed with saturated aqueous NaHCO3 then dried (MgSO4), filtered and evaporated. Trituration with 1:9 EtOAc:isohexanes (10 mL) at reflux followed by cooling to RT afforded a solid which was filtered to afford 1.15 g of the title compound.

후처리

  1. customThe organic layer was separated
  2. washwashed with saturated aqueous NaHCO3
  3. dry with materialthen dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. temperatureTrituration with 1:9 EtOAc:isohexanes (10 mL) at reflux
  7. customafforded a solid which
  8. filtrationwas filtered

출처 및 근거

ORD 기록
ord-38f70e8d280643899a052228c14cb32f
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07906645B2

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