Magnesium Hydroxide → 2-Hydroxyimino-2-(isothiazol-4-yl)acetic acid

HRID 463928

반응식

HRID 463928 반응식
[S:1]1[CH:5]=[C:4]([C:6](=O)[C:7]([OH:9])=[O:8])[CH:3]=[N:2]1.[OH-].[Mg+2].[OH-].[OH:14][NH:15]Cl>C(O)C.O>[OH:14][N:15]=[C:6]([C:4]1[CH:3]=[N:2][S:1][CH:5]=1)[C:7]([OH:9])=[O:8]

참가 물질

6

반응물 3

HCID 73981Magnesium HydroxideHCID 149953Hydroxylamine, N-chloro-HCID 129065552-(Isothiazol-4-yl)glyoxylic acid

생성물 1

HCID 571550852-Hydroxyimino-2-(isothiazol-4-yl)acetic acid수율 76.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A suspension of 2-(isothiazol-4-yl)glyoxylic acid (240 mg.), magnesium hydroxide (290 mg.) and hydroxylamino hydrochloride (140 mg.) in a mixture of ethanol (2 ml.) and water (10 ml.) was stirred for 2 hours at ambient temperature and allowed to stand overnight at ambient temperature. Ethanol was distilled off and to the residue was added ethyl acetate. The mixture was adjusted to pH 1 with 10% hydrochloric acid and the ethyl acetate layer was washed with water and dried over magnesium sulfate. The solvent was distilled off under reduced pressure to give 2-hydroxyimino-2-(isothiazol-4-yl)acetic acid (syn isomer) (0.20 g.), mp 159° to 161° C. (dec.).

후처리

  1. waitto stand overnight at ambient temperature
  2. distillationEthanol was distilled off and to the residue
  3. additionwas added ethyl acetate
  4. washthe ethyl acetate layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-50f6bec9bbb04ee58d9b0c09c574d842
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04544751

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