Bromochloromethane → 5-Chloromethylthio-1-methyltetrazole

HRID 1707426

反応式

HRID 1707426 の反応式
[Na].[CH3:2][N:3]1[C:7]([SH:8])=[N:6][N:5]=[N:4]1.Br[CH2:10][Cl:11]>CN(C)C=O.O>[Cl:11][CH2:10][S:8][C:7]1[N:3]([CH3:2])[N:4]=[N:5][N:6]=1

参加物

5

反応物 2

HCID 6333BromochloromethaneHCID 178482029HCID 178482029、化合物

生成物 1

HCID 103520355-Chloromethylthio-1-methyltetrazole収率 72%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1-methyltetrazole-5-thiol sodium salt (2.00 g: 14.5 mMol.) in dimethylformamide (20 ml) under ice cooling is added bromochloromethane (20 ml) in one portion, and the mixture is stirred for 1.5 hour. The reaction mixture is diluted with water and extracted with ethyl acetate. The extract is washed with brine, dried over sodium sulfate, filtered, and concentrated. The residue is purified by silica gel column chromatography (toluene: ethyl acetate=20:1-10:1) to give 5-chloromethylthio-1-methyltetrazole as colorless crystals (1.73 g). Yield: 72%. m.p. 55° to 56° C.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract is washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue is purified by silica gel column chromatography (toluene: ethyl acetate=20:1-10:1)

出典と根拠

ORDレコード
ord-aa17aa978c944620a9aa9094d688940a
出典データセット
uspto-grants-1994_10
特許番号
US05352792

関連ノート

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