Sodium Hydroxide → 1773508-66-9

HRID 920793노트

반응식

HRID 920793 반응식
[F:1][C:2]1([F:17])[CH2:5][C:4]([C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)([C:6]([O:8]C)=[O:7])[CH2:3]1.[OH-].[Na+]>CO.O.C1COCC1>[F:17][C:2]1([F:1])[CH2:3][C:4]([C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)([C:6]([OH:8])=[O:7])[CH2:5]1

참가 물질

6

반응물 2

HCID 14798Sodium HydroxideHCID 118061145HCID 118061145, 화합물

생성물 1

HCID 1054874861773508-66-9수율 66.3%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of Intermediate 308D (400 mg, 1.638 mmol) in MeOH (5 mL), water (2 mL) and THF (2 mL) was added NaOH (197 mg, 4.91 mmol) and stirred for 12 h at RT. The reaction mixture was concentrated under vacuo and the pH of the residue was adjusted to 2.0 using 1.5 N HCl and the compound was extracted with ethyl acetate (3×10 mL) The combined organic layer was dried over Na2SO4, filtered and the filtrate concentrated under reduced pressure to afford Intermediate 308E as a pale yellow solid (250 mg, 66%). 1H NMR (400 MHz, DMSO-d6) δ ppm 13.03 (bs, 1H), 7.33-7.43 (m, 2H), 7.21 (m, 2H), 3.32-3.37 (m, 2H), 2.99-3.15 (m, 2H).

후처리

  1. concentrationThe reaction mixture was concentrated under vacuo
  2. extractionthe compound was extracted with ethyl acetate (3×10 mL) The combined organic layer
  3. dry with materialwas dried over Na2SO4
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2b4bb4c695b64b0195bfc9410b3d04b1
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09273058B2

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