2,3-Dimethyl-2-butene → 3-Iodo-2-methoxybenzoic acid

HRID 1486180노트

반응식

HRID 1486180 반응식
[I:1][C:2]1[C:3]([O:10][CH3:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].CC(=C(C)C)C.O.P([O-])([O-])(O)=[O:20].[Na+].[Na+].Cl([O-])=O.[Na+]>C(O)(C)(C)C.O.C(OCC)(=O)C>[I:1][C:2]1[C:3]([O:10][CH3:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)[C:5]([OH:20])=[O:6]

참가 물질

8

반응물 4

HCID 112502,3-Dimethyl-2-buteneHCID 61488Phosphoric acid, disodium salt, hydrateHCID 108014193-Iodo-2-methoxybenzaldehydeHCID 23668197Sodium Chlorite

생성물 1

HCID 121684323-Iodo-2-methoxybenzoic acid

시약·촉매·용매 3

HCID 962Water용매HCID 6386tert-Butanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 3-iodo-2-methoxy-benzaldehyde (3.68 g, 14 mmol) in tert-butanol (70 mL) was added 2,3-dimethyl-but-2-ene (7 mL) followed by a solution comprising disodium hydrogen phosphate monohydrate (7.56 g 56 mmol) and sodium chlorite (7.56 g, approx. 66 mmol, technical grade) in water (70 mL). The resulting mixture was stirred for 20 minutes then diluted with ethyl acetate, washed with brine, dried over magnesium sulfate and concentrated. The residual solid was recrystallized from cyclohexane to give the title compound as a white solid.

후처리

  1. washwashed with brine
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residual solid was recrystallized from cyclohexane

출처 및 근거

ORD 기록
ord-793ab56df13b4ab2b4fad41eb28c690d
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422314B2

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