Water → HCID 178521269、化合物

HRID 1395786ノート

反応式

HRID 1395786 の反応式
[OH:1][CH2:2][CH2:3][NH:4][C:5](=[S:8])SC.[N-:9]=[N+:10]=[N-:11].[Na+].O>O1CCOCC1>[OH:1][CH2:2][CH2:3][N:4]1[C:5]([SH:8])=[N:11][N:10]=[N:9]1

参加物

5

反応物 3

HCID 962WaterHCID 33557Sodium AzideHCID 13277332Methyl (2-hydroxyethyl)carbamodithioate

生成物 1

HCID 178521269HCID 178521269、化合物収率 4.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of methyl N-(2-hydroxyethyl)dithiocarbamate (3.7 g.), sodium azide (2.4 g.), water (20 ml.) and dioxane (20 ml.) was heated under reflux for four hours. After the dioxane was removed from the mixture under reduced pressure, the aqueous solution was washed with ether. The solution was adjusted to pH 1 with 10% hydrochloric acid and extracted with ethyl acetate. The extract was concentrated under reduced pressure to give oily product (0.47 g.). The oily product was purified by column chromatography on silica gel to give 1-(2-hydroxyethyl)-1H-tetrazole-5-thiol (0.17 g.). m.p. 135° to 137° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for four hours
  3. customAfter the dioxane was removed from the mixture under reduced pressure
  4. washthe aqueous solution was washed with ether
  5. extractionextracted with ethyl acetate
  6. concentrationThe extract was concentrated under reduced pressure
  7. customto give oily product (0.47 g.)
  8. customThe oily product was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-048e4b2c16414efa996fe87eb4bac4e8
出典データセット
uspto-grants-1980_05
特許番号
US04205166

反応ノート

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