Sodium Hydroxide → HCID 54111090、化合物

HRID 1438706ノート

反応式

HRID 1438706 の反応式
I.[CH3:2][NH:3][C:4](=[NH:7])[S:5][CH3:6].[CH3:8][N:9]([C:13](Cl)=[O:14])[C:10](Cl)=[O:11].[OH-].[Na+]>C1C=CC=CC=1.O>[CH3:8][N:9]1[C:13](=[O:14])[NH:7][CH:4]([S:5][CH3:6])[N:3]([CH3:2])[C:10]1=[O:11]

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 15555334N-methyl-bis-(chlorocarbonyl)-amineHCID 178485204HCID 178485204、化合物

生成物 1

HCID 54111090HCID 54111090、化合物収率 75%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回HCID 962Water溶媒2 回

実験手順

23.2 g (0.1 mole) of N,S-dimethyl-isothiourea hydroiodide were initially introduced into 100 ml of water and 250 ml of benzene. 15.6 (0.1 mole) of N-methyl-bis-(chlorocarbonyl)-amine in 100 ml of dry benzene and 12 g (0.3 mole) of sodium hydroxide dissolved in 100 ml of water were simultaneously slowly added dropwise from two dropping funnels with vigorous stirring. The reaction took place strongly exothermically. The mixture was stirred for a further hour, any product which precipitated was filtered off, and the benzene phase was separated off, dried over calcium chloride and evaporated in vacuo. The residue, together with the filter residue, was recrystallized from isopropanol. 14 g (75%) of 1,3-dimethyl-4-methylmercapto tetrahydro-1,3,5-triazine-2,6-dione were obtained as a colorless powder of melting point 137°-139° C.

後処理

  1. additionwere simultaneously slowly added dropwise from two dropping funnels with vigorous stirring
  2. customany product which precipitated
  3. filtrationwas filtered off
  4. customthe benzene phase was separated off
  5. dry with materialdried over calcium chloride
  6. customevaporated in vacuo
  7. customThe residue, together with the filter residue, was recrystallized from isopropanol

出典と根拠

ORDレコード
ord-c7d9cbe858c14bb4b92146e20d59c3b3
出典データセット
uspto-grants-1977_11
特許番号
US04056527

反応ノート

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