Hydrochloric Acid → N-(2-Hydroxy-4-octyloxy-phenyl)-2,2,2-trifluoro-acetamide

HRID 18447

반응식

HRID 18447 반응식
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10](=[O:15])[C:11]([F:14])([F:13])[F:12].C([O-])([O-])=O.[K+].[K+].Br[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30].Cl>CN(C=O)C>[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH:5]=[CH:4][C:3]=1[NH:9][C:10](=[O:15])[C:11]([F:12])([F:13])[F:14]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 81401-BromooctaneHCID 11430Potassium CarbonateHCID 18454996N-(2,4-dihydroxyphenyl)-2,2,2-trifluoro-acetamide

생성물 1

HCID 58685869N-(2-Hydroxy-4-octyloxy-phenyl)-2,2,2-trifluoro-acetamide수율 82.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of N-(2,4-dihydroxy phenyl)-2,2,2-trifluoro-acetamide (0.44 g; 2 mmol) in DMF (4 mL) was added K2CO3 and 1-bromooctane (0.37 mL; 2.1 mmol). The slurry was stirred for 2 days at room temperature, poured onto 0.1 M HCl (aq.; 50 mL) and then extracted with diethylether (30 mL). The organic phase was dried (MgSO4), filtered and the eluate evaporated to leave 550 mg of black solid which was purified by chromatography (SiO2; PE80-100° C./EtOAc=4:1) to leave 100 mg (15%) of a pure white solid. Mp. 114-116° C.; MS (GC-MS; Cl): 334 (MH+).

후처리

  1. extractionextracted with diethylether (30 mL)
  2. dry with materialThe organic phase was dried (MgSO4)
  3. filtrationfiltered
  4. customthe eluate evaporated

출처 및 근거

ORD 기록
ord-4ee9517eb9ec420cb4980422cdb446dd
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741352B2

연결된 노트

불러오는 중…