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Sodium Hydroxide → HCID 178526006、化合物

HRID 904868
ノート
印刷プレビュー

反応式

HRID 904868 の反応式
[C:1]([CH2:6][N:7]1[C:11]([SH:12])=[N:10][N:9]=[N:8]1)([C:3]([OH:5])=[O:4])=[O:2].[OH-].[Na+]>C(O)C.[Zn]>[C:3]([CH:1]([OH:2])[CH2:6][N:7]1[C:11]([SH:12])=[N:10][N:9]=[N:8]1)([OH:5])=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 178526005HCID 178526005、化合物

生成物 1

HCID 178526006HCID 178526006、化合物収率 42.1%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 702Ethanol溶媒

実験手順

1-Oxalomethyl-1H-tetrazole-5-thiol (0.94 g) was dissolved in aqueous 60% ethanol (15 ml) containing sodium hydroxide (1.4 g) and to this solution was added portionwise zinc powder (0.98 g). The mixture was stirred at room temperature for 3.5 hours. After removal of zinc powder by filtration, ethanol was removed under reduced pressure and the remained aqueous solution was adjusted to pH 2.0 with 10% hydrochloric acid. Extraction with ethyl acetate, drying over magnesium sulfate and evaporation gave an oil which was triturated with a mixture of diisopropyl ether and n-hexane (1:1). The crystals were filtered and washed with a mixture of diisopropyl ether and n-hexane (1:1) to give 1-(2-carboxy-2-hydroxyethyl)-1H-tetrazole-5-thiol (0.40 g), mp 143° to 146° C.,

後処理

  1. customAfter removal of zinc powder
  2. filtrationby filtration, ethanol
  3. customwas removed under reduced pressure
  4. extractionExtraction with ethyl acetate
  5. dry with materialdrying over magnesium sulfate and evaporation
  6. customgave an oil which
  7. customwas triturated with a mixture of diisopropyl ether and n-hexane (1:1)
  8. filtrationThe crystals were filtered
  9. washwashed with a mixture of diisopropyl ether and n-hexane (1:1)

出典と根拠

ORDレコード
ord-f2c48d0e1e7a47618fdc41b2e1a91011
出典データセット
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04420477

反応ノート

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