Water → HCID 178525591、化合物

HRID 895056ノート

反応式

HRID 895056 の反応式
[C:1]([CH2:4][CH2:5][NH:6][C:7](=[S:10])SC)([OH:3])=[O:2].[OH-].[Na+].O.[N-:14]=[N+:15]=[N-:16].[Na+]>CCOCC>[C:1]([CH2:4][CH2:5][N:6]1[C:7]([SH:10])=[N:16][N:15]=[N:14]1)([OH:3])=[O:2]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 33557Sodium AzideHCID 12458601Methyl 2-carboxyethyldithiocarbamate

生成物 1

HCID 178525591HCID 178525591、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a mixture of 25.37 g. (0.143 mol.) of methyl 2-carboxyethyldithiocarbamate and 5.6 g. (0.143 mol.) of sodium hyroxide in 210 ml. of water was added 9.25 g. (0.143 mol.) of sodium azide. The reaction mixture was refluxed for one hour then cooled, diluted with 100 ml. of ether and acidified to pH 1.7. The layers were separated, the aqueous phase was extracted with ether and the combined extracts were dried (MgSO4) and evaporated to dryness to give a residue which was recrystallized from acetone-chloroform to give 1-(2-carboxyethyl)tetrazole-5-thiol, m.p. 158°-160°.

後処理

  1. additionTo a mixture of 25.37 g
  2. temperatureThe reaction mixture was refluxed for one hour
  3. temperaturethen cooled
  4. additiondiluted with 100 ml
  5. customThe layers were separated
  6. extractionthe aqueous phase was extracted with ether
  7. dry with materialthe combined extracts were dried (MgSO4)
  8. customevaporated to dryness
  9. customto give a residue which
  10. customwas recrystallized from acetone-chloroform

出典と根拠

ORDレコード
ord-00cb9cac598b407ebdd21d21453d6f6f
出典データセット
uspto-grants-1981_08
特許番号
US04286089

反応ノート

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