Methane → HCID 178427298, 화합물

HRID 1704196

반응식

HRID 1704196 반응식
[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

참가 물질

7

반응물 5

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

생성물 1

HCID 178427298HCID 178427298, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-ab7a75f7cb834f6bb853c2f1e5493b78
출처 데이터셋
uspto-grants-1978_11
특허 번호
US04126590

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