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Sodium Hydroxide → 2,4-Dichloro-3-(3-methylisoxazol-5-yl)benzoic acid

HRID 1276138
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HRID 1276138 반응식
[OH-].[Na+].[Cl:3][C:4]1[C:13]([C:14]2[O:18][N:17]=[C:16]([CH3:19])[CH:15]=2)=[C:12]([Cl:20])[CH:11]=[CH:10][C:5]=1[C:6]([O:8]C)=[O:7]>O.CO.O1CCCC1>[Cl:3][C:4]1[C:13]([C:14]2[O:18][N:17]=[C:16]([CH3:19])[CH:15]=2)=[C:12]([Cl:20])[CH:11]=[CH:10][C:5]=1[C:6]([OH:8])=[O:7]
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참가 물질

6

반응물 2

HCID 14798Sodium HydroxideHCID 15430825Methyl 2,4-dichloro-3-(3-methylisoxazol-5-yl)benzoate

생성물 1

HCID 154308262,4-Dichloro-3-(3-methylisoxazol-5-yl)benzoic acid수율 96.5%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran
용매

실험 절차

0.35 g (8.8 mmol) of sodium hydroxide in 35 ml of water was added to 2.3 g (8.0 mmol) of methyl 2,4-dichloro-3-(3-methylisoxazol-5-yl)benzoate in a mixture of 50 ml of methanol and 50 ml of tetrahydrofuran. The mixture was stirred at room temperature for 12 hours, the solvent was removed and the residue was taken up in ethyl acetate/water. After phase separation, the organic phase was separated off and the aqueous phase was washed with ethyl acetate. The remaining aqueous phase was acidified and then extracted with ethyl acetate; the resulting organic phase was dried and concentrated. 2.1 g (96% of theory) of 2,4-dichloro-3-(3-methylisoxazol-5-yl)benzoic acid were obtained.

후처리

  1. customthe solvent was removed
  2. customAfter phase separation
  3. customthe organic phase was separated off
  4. washthe aqueous phase was washed with ethyl acetate
  5. extractionextracted with ethyl acetate
  6. customthe resulting organic phase was dried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-84e1a5d0ea024f33a9d47a544dfed830
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06165944

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