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Sodium Hydroxide → 2-Chloro-3-(5-methyl-4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoic acid

HRID 1276117
ノート
印刷プレビュー

反応式

HRID 1276117 の反応式
[OH-].[Na+].[Cl:3][C:4]1[C:13]([C:14]2[CH2:18][CH:17]([CH3:19])[O:16][N:15]=2)=[C:12]([S:20]([CH3:23])(=[O:22])=[O:21])[CH:11]=[CH:10][C:5]=1[C:6]([O:8]C)=[O:7]>CO>[Cl:3][C:4]1[C:13]([C:14]2[CH2:18][CH:17]([CH3:19])[O:16][N:15]=2)=[C:12]([S:20]([CH3:23])(=[O:21])=[O:22])[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

4

反応物 2

HCID 14798Sodium HydroxideHCID 22114913Methyl 2-chloro-(5-methyl-4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoate

生成物 1

HCID 221149242-Chloro-3-(5-methyl-4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoic acid収率 92.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A solution of 3.52 g (88 mmol) of sodium hydroxide in 100 ml of methanol was slowly added dropwise to a mixture of 15.00 g (45 mmol) of methyl 2-chloro-3-(5-methyl-4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoate and 200 ml of methanol. The suspension was stirred at room temperature for 48 hours. The solvent was distilled off, the residue was taken up in water and the aqueous phase was washed three times with ethyl acetate. The aqueous phase was acidified with hydrochloric acid and extracted three times with ethyl acetate. The combined organic phases were subsequently washed neutral with water, dried and concentrated. 13.20 g (92% of theory) of 2-chloro-3-(5-methyl-4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoic acid were obtained.

後処理

  1. distillationThe solvent was distilled off
  2. washthe aqueous phase was washed three times with ethyl acetate
  3. extractionextracted three times with ethyl acetate
  4. customdried
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-b58a97322472437cac0737fe50f10f9d
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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