Potassium Hydroxide → HCID 86611483、化合物

HRID 1444917ノート

反応式

HRID 1444917 の反応式
Cl.[NH2:2][OH:3].[OH-].[K+].CO[C:8](=[O:33])[C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH2:19][C:18]([C:24]3[CH:29]=[C:28]([Cl:30])[CH:27]=[C:26]([Cl:31])[CH:25]=3)([C:20]([F:23])([F:22])[F:21])[O:17][N:16]=2)=[CH:11][C:10]=1[CH3:32]>CO>[Cl:30][C:28]1[CH:29]=[C:24]([C:18]2([C:20]([F:23])([F:21])[F:22])[O:17][N:16]=[C:15]([C:12]3[CH:13]=[CH:14][C:9]([C:8]([NH:2][OH:3])=[O:33])=[C:10]([CH3:32])[CH:11]=3)[CH2:19]2)[CH:25]=[C:26]([Cl:31])[CH:27]=1

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 59563501Methyl 4-(5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazol-3-yl)-2-methylbenzoate

生成物 1

HCID 86611483HCID 86611483、化合物収率 100.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

反応条件

温度
40 °C

実験手順

In a solution of 0.30 g of hydroxylamine hydrochloride in 10 ml of methanol, a solution of 0.65 g of potassium hydroxide in 5 ml of methanol was added, then a solution of 1.00 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methylbenzoic acid methyl ester synthesized similarly to Steps 1 to 4 of Synthetic Example 28 in 10 ml of methanol was added, and stirred at 40° C. for 1 hour. After the completion of the reaction, the solvent was distilled off under reduced pressure, 10 ml of acetic acid aqueous solution (1:1) was added in the residue, and extracted with ethyl acetate (20 ml×2), the organic phase was dehydrated and dried with saturated sodium chloride aqueous solution and anhydrous sodium sulfate in that order, and the solvent was distilled under reduced pressure. Toluene was added in the residue and the remaining acetic acid was distilled off azeotropically to obtain 1.01 g of crude 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methylbenzhydroxamic acid as white crystal.

後処理

  1. additionwas added
  2. customAfter the completion of the reaction
  3. distillationthe solvent was distilled off under reduced pressure, 10 ml of acetic acid aqueous solution (1:1)
  4. additionwas added in the residue
  5. extractionextracted with ethyl acetate (20 ml×2)
  6. dry with materialdried with saturated sodium chloride aqueous solution and anhydrous sodium sulfate in that order
  7. distillationthe solvent was distilled under reduced pressure
  8. additionToluene was added in the residue
  9. distillationthe remaining acetic acid was distilled off azeotropically

出典と根拠

ORDレコード
ord-7df42f0a4a8c4147a693d769a0fbeda0
出典データセット
uspto-grants-2010_02
特許番号
US07662972B2

反応ノート

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