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

HRID 1276138
ノート
印刷プレビュー

反応式

HRID 1276138 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-84e1a5d0ea024f33a9d47a544dfed830
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06165944

反応ノート

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