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

HRID 463928

反応式

HRID 463928 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-50f6bec9bbb04ee58d9b0c09c574d842
出典データセット
uspto-grants-1985_10
特許番号
US04544751

関連ノート

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