Methanethiol → 2-Chloro-6-(methylsulfanyl)pyrazine

HRID 1679661ノート

反応式

HRID 1679661 の反応式
[Na].[H-].[Na+].[CH3:4][SH:5].[Cl:6][C:7]1[CH:12]=[N:11][CH:10]=[C:9](Cl)[N:8]=1>C1C=CC=CC=1>[Cl:6][C:7]1[CH:12]=[N:11][CH:10]=[C:9]([S:5][CH3:4])[N:8]=1

参加物

6

反応物 4

HCID 878MethanethiolHCID 24758Sodium hydrideHCID 785042,6-DichloropyrazineHCID 5360545Sodium

生成物 1

HCID 203616852-Chloro-6-(methylsulfanyl)pyrazine

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 0.13 mole of sodium methylmercaptide (prepared from 3.12 g. sodium hydride and excess methyl mercaptan), 20 g. (0.13 mole) of 2,6-dichloropyrazine and 200 ml. benzene is heated at reflux for 24 hours, cooled and washed twice with 50 ml. water. The benzene layer is separated, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. Distillation of the residue gives 2-chloro-6-methylthiopyrazine.

後処理

  1. temperatureat reflux for 24 hours
  2. temperaturecooled
  3. washwashed twice with 50 ml
  4. customThe benzene layer is separated
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. distillationDistillation of the residue

出典と根拠

ORDレコード
ord-51ce95e9ccca438d8bee797a9daa1d48
出典データセット
uspto-grants-1978_03
特許番号
US04081542

反応ノート

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