Hydroxyamine hydrochloride → HCID 73508098, 화합물

HRID 2259651노트

반응식

HRID 2259651 반응식
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]

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 15342529HCID 15342529, 화합물

생성물 1

HCID 73508098HCID 73508098, 화합물수율 101.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-98c84408806d4feeb0670a114455b46e
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05475014

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