Methane → HCID 178427298、化合物

HRID 1704196

反応式

HRID 1704196 の反応式
[C:1]1([CH3:13])[CH:6]=[CH:5][C:4]([S:7]([CH2:10][C:11]#[N:12])(=[O:9])=[O:8])=[CH:3][CH:2]=1.[N-:14]=[N+:15]=[N-:16].[Na+].[Cl-].[NH4+].C.Cl>CN(C)C=O>[C:1]1([CH3:13])[CH:2]=[CH:3][C:4]([S:7]([CH2:10][C:11]2[NH:16][N:15]=[N:14][N:12]=2)(=[O:8])=[O:9])=[CH:5][CH:6]=1

参加物

7

反応物 5

HCID 297MethaneHCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 79776Tosylacetonitrile

生成物 1

HCID 178427298HCID 178427298、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

97.5 parts of p-tolylsulphonyl-acetonitrile are stirred together with 39 parts of sodium azide, 32 parts of ammonium chloride and 200 parts of dimethylformamide for 10 hours at 120°-130° C. The dimethylformamide is distilled off in vacuo, and the residue is dissolved in 1000 parts of water with the addition of sodium hydroxide to give pH 9. The solution is treated with animal charcoal, and precipitation is effected at pH 2-3 by the addition of hydrochloric acid. Recrystallisation of the precipitate from isopropanol yields 85 parts of 5-(p-tolylsulphonylmethyl)-tetrazole in the form of white crystals which melt at 206°-208°.

後処理

  1. distillationThe dimethylformamide is distilled off in vacuo
  2. dissolutionthe residue is dissolved in 1000 parts of water with the addition of sodium hydroxide
  3. customto give pH 9
  4. customRecrystallisation of the precipitate from isopropanol

出典と根拠

ORDレコード
ord-ab7a75f7cb834f6bb853c2f1e5493b78
出典データセット
uspto-grants-1978_11
特許番号
US04126590

関連ノート

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