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Hydrochloric Acid → HCID 178526005、化合物

HRID 1380689
ノート
印刷プレビュー

反応式

HRID 1380689 の反応式
[C:1]([CH2:8][N:9]1[C:13]([SH:14])=[N:12][N:11]=[N:10]1)([C:3]([O:5]CC)=[O:4])=[O:2].[OH-].[Na+].Cl>CO>[C:1]([CH2:8][N:9]1[C:13]([SH:14])=[N:12][N:11]=[N:10]1)([C:3]([OH:5])=[O:4])=[O:2]
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 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178473105HCID 178473105、化合物

生成物 1

HCID 178526005HCID 178526005、化合物収率 59.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 1-ethoxalylmethyl-1H-tetrazole-5-thiol (18.6 g) in methanol (186 ml) was added 1N aqueous solution of sodium hydroxide (172 ml) at room temperature and the mixture was stirred for 40 minutes. After adjusting to pH 7.5 with 10% hydrochloric acid, the solution was evaporated in vacuo to remove methanol and the remained aqueous solution was washed with ethyl acetate (100 ml). The aqueous solution was adjusted to pH 4.0 and washed again with ethyl acetate to remove impurities. The aqueous solution was adjusted to pH 2.5, and extracted with ethyl acetate, dried over magnesium sulfate and evaporated to give pale yellow powder of 1-oxalomethyl-1H-tetrazole-5-thiol (9.7 g), mp 140° to 150° C. (dec.).

後処理

  1. customthe solution was evaporated in vacuo
  2. customto remove methanol
  3. washthe remained aqueous solution was washed with ethyl acetate (100 ml)
  4. washwashed again with ethyl acetate
  5. customto remove impurities
  6. extractionextracted with ethyl acetate
  7. dry with materialdried over magnesium sulfate
  8. customevaporated

出典と根拠

ORDレコード
ord-0fd3b5d239df4c618fa4b809ddcadba0
出典データセット
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04582908

反応ノート

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