Lithium hydroxide, monohydrate → HCID 59483858、化合物

HRID 1808384ノート

反応式

HRID 1808384 の反応式
O.[OH-].[Li+].[Cl:4][C:5]1[CH:6]=[C:7]([NH:12][C:13]([N:15]2[CH2:20][CH2:19][C:18]3[O:21][N:22]=[C:23]([C:24]([O:26]CC)=[O:25])[C:17]=3[CH2:16]2)=[O:14])[CH:8]=[CH:9][C:10]=1[Cl:11]>O.CO>[Cl:4][C:5]1[CH:6]=[C:7]([NH:12][C:13]([N:15]2[CH2:20][CH2:19][C:18]3[O:21][N:22]=[C:23]([C:24]([OH:26])=[O:25])[C:17]=3[CH2:16]2)=[O:14])[CH:8]=[CH:9][C:10]=1[Cl:11]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 59483856Ethyl 5-(3,4-dichlorophenylcarbamoyl)-4,5,6,7-tetrahydroisoxazolo[4,5-c]pyridine-3-carboxylate

生成物 1

HCID 59483858HCID 59483858、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Lithium hydroxide monohydrate (56%) (0.25 g, 6.038 mmol) dissolved in water (8 ml) was added to a solution of ethyl 5-(3,4-dichlorophenylcarbamoyl)-4,5,6,7-tetrahydroisoxazolo[4,5-c]pyridine-3-carboxylate (1.2 g, 3.019 mmol) in methanol (25 ml), and the mixture was stirred for 15 h. The solvent was removed in vacuo. The aqueous phase was adjusted to an acidic pH value with dilute HCl solution (aq.) and extracted with ethyl acetate. The organic phase was dried over sodium sulfate, filtered and concentrated in vacuo. The resulting crude product was used directly in the following stage. Yield: 0.94 g (87%).

後処理

  1. customThe solvent was removed in vacuo
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-46649ce0f1f143cd8a068557ede36be5
出典データセット
uspto-grants-2013_01
特許番号
US08357717B2

反応ノート

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