Carbon Dioxide → 3,6-Difluoro-2-methoxybenzoic acid

HRID 508189노트

반응식

HRID 508189 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[O:9][CH3:10].[Li+].CC([N-]C(C)C)C.[Li]CCCC.C(NC(C)C)(C)C.[C:31](=[O:33])=[O:32].OS(O)(=O)=O>C1COCC1.C(OCC)C>[F:1][C:2]1[C:3]([O:9][CH3:10])=[C:4]([C:5]([F:8])=[CH:6][CH:7]=1)[C:31]([OH:33])=[O:32]

참가 물질

9

반응물 6

HCID 280Carbon DioxideHCID 1118Sulfuric AcidHCID 7912DiisopropylamineHCID 2724682Lithium diisopropylamideHCID 27249892,5-DifluoroanisoleHCID 178418339Butyllithium

생성물 1

HCID 160942453,6-Difluoro-2-methoxybenzoic acid

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 1,4-difluoro-2-methoxybenzene (i-6a) (2.88 g, 20 mmol) in THF (5 mL) was added to a solution of LDA freshly prepared from n-BuLi (10M solution in hexane, 2.2 mL, 22 mmol) and diisopropylamine (2.28 g, 22.8 mmol) in THF (20 mL) at −60° C. After 30 min, a freshly prepared solution of CO2 in diethyl ether (20 mL) was quickly added. Then aq. H2SO4 was added, and the resulting precipitate was collected and washed with H2O, and dried to give the title compound (i-6b) as white crystals. LCMS (ESI) calc'd for C8H6F2O3 [M+H]+: 189. found: 189.

후처리

  1. customthe resulting precipitate was collected
  2. washwashed with H2O
  3. customdried

출처 및 근거

ORD 기록
ord-5aafd660425941529d5bb7699d4bd151
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09095583B2

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