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Dichloromethane → 5-Acetonylthio-1,4-dimethyltetrazolium chloride

HRID 728032
ノート
印刷プレビュー

反応式

HRID 728032 の反応式
[CH2:1]([S:5][C:6]1[N:10]([CH3:11])[N:9]=[N:8][N:7]=1)[C:2]([CH3:4])=[O:3].F[C:13](F)(F)S(OC)(=O)=O.C(Cl)[Cl:22]>CO>[Cl-:22].[CH2:1]([S:5][C:6]1[N:10]([CH3:11])[N:9]=[N:8][N+:7]=1[CH3:13])[C:2]([CH3:4])=[O:3]
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 6344DichloromethaneHCID 9526Methyl triflateHCID 30619772-Propanone, 1-((1-methyl-1H-tetrazol-5-yl)thio)-

生成物 1

HCID 150071015-Acetonylthio-1,4-dimethyltetrazolium chloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

The 5-acetonylthio-1-methyltetrazole, prepared as above described, was dissolved in 20 ml of methylene chloride and to the resulting solution was added 0.617 gram (0.0055 mol) of methyl trifluoromethanesulfonate and the mixture allowed to stand overnight at room temperature. Thereafter, the solvent was vaporized off and an oily residue obtained. The latter was dissolved in aqueous methanol and the methanol solution passed over a Dowex-1 (Cl-) ion exchange column. The eluate from the column was evaporated to obtain a waxy material which was triturated with hexane to obtain a waxy solid which after drying in high vacuum amounted to 0.80 gram of 5-acetonylthio-1,4-dimethyltetrazolium chloride, m.p. 102°-104° C.

後処理

  1. customan oily residue obtained
  2. customThe eluate from the column was evaporated
  3. customto obtain a waxy material which
  4. customwas triturated with hexane
  5. customto obtain a waxy solid which
  6. customafter drying in high vacuum

出典と根拠

ORDレコード
ord-ebf58799f27d43c88fd0ee0127a3dc64
出典データセット
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05047416

反応ノート

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