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Sodium Hydroxide → 2-Methoxyimino-2-(1,2,3-thiadiazol-4-yl)acetic acid

HRID 435226
ノート
印刷プレビュー

反応式

HRID 435226 の反応式
[OH-].[Na+].[CH3:3][O:4][N:5]=[C:6]([C:12]1[N:13]=[N:14][S:15][CH:16]=1)[C:7]([O:9]CC)=[O:8]>CO>[CH3:3][O:4][N:5]=[C:6]([C:12]1[N:13]=[N:14][S:15][CH:16]=1)[C:7]([OH:9])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 53899707Ethyl 2-methoxyimino-2-(1,2,3-thiadiazol-4-yl)acetate

生成物 1

HCID 543473402-Methoxyimino-2-(1,2,3-thiadiazol-4-yl)acetic acid収率 67.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1 N Aqueous solution of sodium hydroxide (6.7 ml.) was added to a solution of ethyl 2-methoxyimino-2-(1,2,3-thiadiazol-4-yl)acetate (syn isomer) (1.2 g.) in methanol (10 ml.) and the mixture was stirred for 1.5 hours at ambient temperature. Methanol was distilled off from the reaction mixture and water was added to the residue. The mixture was washed with ether, adjusted to pH 1 with 10% hydrochloric acid and extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. The solvent was distilled off to give prisms of 2-methoxyimino-2-(1,2,3-thiadiazol-4-yl)acetic acid (syn isomer) (0.7 g.), m.p. 110° to 113° C.

後処理

  1. distillationMethanol was distilled off from the reaction mixture and water
  2. additionwas added to the residue
  3. washThe mixture was washed with ether
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with a saturated aqueous solution of sodium chloride
  6. dry with materialdried over magnesium sulfate
  7. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-202215536bf64714be612b78ef086a24
出典データセット
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04400379

反応ノート

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