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HCID 14722309、化合物 → HCID 10620577、化合物

HRID 1031680
ノート
印刷プレビュー

反応式

HRID 1031680 の反応式
C([O:8][C:9]1[CH:22]=[C:21]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[C:20]([O:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[CH:19][C:10]=1[C:11]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:12])C1C=CC=CC=1>C(O)C.[C].[Pd]>[OH:8][C:9]1[CH:22]=[C:21]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[C:20]([O:28][C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)=[CH:19][C:10]=1[C:11]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:12]
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 1

HCID 14722309HCID 14722309、化合物

生成物 1

HCID 10620577HCID 10620577、化合物収率 88%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

In 50 ml of ethanol was dissolved 4.83 g of ethyl 2-(2-benzyloxy-4-methylsulfonylamino-5-phenoxybenzoyl)acetate. Thereto was added 200 mg of 5% palladium-carbon. The mixture was subjected to hydrogenation for 1 hour at 40° C. at atmospheric pressure. After the completion of the reaction, the catalyst was removed by filtration. The filtrate was subjected to distillation under reduced pressure to remove the solvent. The residue was mixed with diisopropyl ether. The resulting crystal was collected by filtration and recrystallized from a mixed solvent of ethyl acetate and diisopropyl ether to obtain 3.46 g (yield: 88%) of ethyl 2-(2-hydroxy-4-methylsulfonylamino-5-phenoxybenzoyl)acetate having a melting point of 111.5°-112.5° C.

後処理

  1. customAfter the completion of the reaction
  2. customthe catalyst was removed by filtration
  3. distillationThe filtrate was subjected to distillation under reduced pressure
  4. customto remove the solvent
  5. additionThe residue was mixed with diisopropyl ether
  6. filtrationThe resulting crystal was collected by filtration
  7. customrecrystallized from a mixed solvent of ethyl acetate and diisopropyl ether

出典と根拠

ORDレコード
ord-1eed135637b34bfcba7753e0594d2d0b
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04954518

反応ノート

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