Triethylamine → HCID 53804495、化合物

HRID 1438698ノート

反応式

HRID 1438698 の反応式
[CH3:1][N:2]([C:6](Cl)=[O:7])[C:3](Cl)=[O:4].I.[CH3:10][S:11][C:12](=[NH:18])[NH:13][N:14]=[C:15]([CH3:17])[CH3:16].C(N(CC)CC)C>C1C=CC=CC=1>[CH3:1][N:2]1[C:6](=[O:7])[NH:18][CH:12]([S:11][CH3:10])[N:13]([N:14]=[C:15]([CH3:17])[CH3:16])[C:3]1=[O:4]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 15555334N-methyl-bis-(chlorocarbonyl)-amineHCID 178504061HCID 178504061、化合物

生成物 1

HCID 53804495HCID 53804495、化合物収率 76%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒3 回

実験手順

15.6 g (0.1 mole) of N-methyl-bis-(chlorocarbonyl)-amine were dissolved in 100 ml of benzene and added dropwise, whilst stirring, to 27.3 g (0.1 mole) of acetone-S-methyliso-thio-semicarbazone hydroiodide suspended in 100 ml of benzene. Thereafter, 30.3 g (0.3 mole) of triethylamine in 50 ml of benzene were slowly added dropwise. The mixture was stirred for a further hour and the precipitate was filtered off. The precipitate was introduced into 100 ml of chloroform and 100 ml of water and extracted by shaking. The chloroform phase was separated off, dried over calcium chloride and evaporated in vacuo, together with the benzene filtrate. The resudue was recrystallized from isopropanol. 17.3 g (76%) of 1-methyl-3-isopropylideneamino-4-methylmercapto-tetrahydro-1,3,5-triazine-2,6-dione were obtained as a colorless powder; melting point 130-132° C.

後処理

  1. additionadded dropwise
  2. filtrationthe precipitate was filtered off
  3. additionThe precipitate was introduced into 100 ml of chloroform and 100 ml of water
  4. extractionextracted
  5. stirringby shaking
  6. customThe chloroform phase was separated off
  7. dry with materialdried over calcium chloride
  8. customevaporated in vacuo, together with the benzene filtrate
  9. customThe resudue was recrystallized from isopropanol

出典と根拠

ORDレコード
ord-b0d566ef6d0f4810b43a904e84fdc2a9
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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