Hydroxyamine hydrochloride → HCID 73508098、化合物

HRID 2259651ノート

反応式

HRID 2259651 の反応式
OC1[O:6][CH:5]([C:7]2[S:8][C:9]3[CH:15]=[C:14]([N:16]4[CH2:20][CH:19]([CH2:21][O:22][CH3:23])[O:18][C:17]4=[O:24])[CH:13]=[CH:12][C:10]=3[N:11]=2)[CH2:4][CH2:3]1.Cl.[NH2:26][OH:27]>N1C=CC=CC=1>[OH:6][CH:5]([C:7]1[S:8][C:9]2[CH:15]=[C:14]([N:16]3[CH2:20][CH:19]([CH2:21][O:22][CH3:23])[O:18][C:17]3=[O:24])[CH:13]=[CH:12][C:10]=2[N:11]=1)[CH2:4][CH:3]=[N:26][OH:27]

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 15342529HCID 15342529、化合物

生成物 1

HCID 73508098HCID 73508098、化合物収率 101.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

72 g of the 3-[2-(5-hydroxytetrahydrofuran-2-yl)-benzothiazol-6-yl]-5-methoxymethyl-2-oxazolidinone obtained in the Example 7 was dissolved in 150 ml of pyridine. 18.6 g of hydroxylamine hydrochloride was added to the solution at room temperature and the mixture was stirred for 10 min and then poured into ice/water. After extraction with ethyl acetate followed by washing with dilute hydrochloric acid, an aqueous sodium hydrogencarbonate solution and an aqueous common salt solution, the product was dried over magnesium sulfate. After concentration under reduced pressure, the obtained solid was recrystallized from acetone/diisopropyl ether to give 73 g of the titled compound.

後処理

  1. extractionAfter extraction with ethyl acetate
  2. washby washing with dilute hydrochloric acid
  3. dry with materialan aqueous sodium hydrogencarbonate solution and an aqueous common salt solution, the product was dried over magnesium sulfate
  4. concentrationAfter concentration under reduced pressure
  5. customthe obtained solid was recrystallized from acetone/diisopropyl ether

出典と根拠

ORDレコード
ord-98c84408806d4feeb0670a114455b46e
出典データセット
uspto-grants-1995_12
特許番号
US05475014

反応ノート

読み込み中…