Ammonium Chloride → HCID 14001754, 화합물

HRID 243820노트

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HRID 243820 반응식
FC(F)(F)S(O[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][CH3:14])[CH:8]=1)(=O)=O.[CH2:17]([Mg]Br)[CH:18]([CH3:20])[CH3:19].[Cl-].[NH4+]>O1CCCC1.CN1CCCC1=O.C/C(/[O-])=C\C(C)=O.C/C(/[O-])=C\C(C)=O.C/C(/[O-])=C\C(C)=O.[Fe+3]>[CH2:17]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][CH3:14])[CH:8]=1)[CH:18]([CH3:20])[CH3:19]

참가 물질

7

반응물 3

HCID 25517Ammonium ChlorideHCID 5656333-Methoxyphenyl trifluoromethanesulfonateHCID 178418816HCID 178418816, 화합물

생성물 1

HCID 14001754HCID 14001754, 화합물

시약·촉매·용매 3

HCID 53384555HCID 53384555, 화합물촉매HCID 8028Tetrahydrofuran용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

To a solution of the compound (2 g) prepared in Example 32 in tetrahydrofuran (35 mL), 1-methyl-2-pyrrolidone (5.2 mL), tris(2,4-pentanedionato)iron(III) (413.5 mg), and isobutyl magnesium bromide (2M diethyl ether solution, 4.68 mL) were added thereto, followed by stirring at room temperature for 4 hours. The reaction mixture was added with a saturated aqueous ammonium chloride solution and the mixture was extracted with t-butyl methyl ether. The organic layer was successively washed with a saturated aqueous ammonium chloride solution, water, and brine, dried and concentrated. Thus, the obtained residue was purified by silica gel column chromatography (hexane:tetrahydrofuran=50:1 to 20:1) to thereby give the title compound (922.5 mg) having the following physical properties.

후처리

  1. extractionthe mixture was extracted with t-butyl methyl ether
  2. washThe organic layer was successively washed with a saturated aqueous ammonium chloride solution, water, and brine
  3. customdried
  4. concentrationconcentrated
  5. customThus, the obtained residue was purified by silica gel column chromatography (hexane:tetrahydrofuran=50:1 to 20:1)

출처 및 근거

ORD 기록
ord-5a3c78d7cbe04c37844b3b2c00793a90
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653305B2

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