Methylamine → HCID 178485068、化合物

HRID 1380150ノート

反応式

HRID 1380150 の反応式
O.[C:2]([NH:4][C:5](=[N:8][CH2:9][CH2:10][S:11][CH2:12][C:13]1[N:14]=[CH:15][NH:16][C:17]=1[CH3:18])SC)#[N:3].[CH3:19][NH2:20]>O>[CH3:19][NH:20][C:5]([NH:8][CH2:9][CH2:10][S:11][CH2:12][C:13]1[N:14]=[CH:15][NH:16][C:17]=1[CH3:18])=[N:4][C:2]#[N:3]

参加物

4

反応物 2

HCID 6329MethylamineHCID 20242239N-cyano-N'-{2-[(5-methylimidazol-4-yl)-methylthio]-ethyl}-S-methylisothiourea monohydrate

生成物 1

HCID 178485068HCID 178485068、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

N-cyano-N'-{2-[(5-methylimidazol-4-yl)-methylthio]-ethyl}-S-methylisothiourea monohydrate (14.35 g; 0.05 mole) is suspended in distilled water (50 ml), stirred and heated. At a bath temperature of 50° C., aqueous methylamine solution (18.5 ml containing 411 g/liter of methylamine, i.e. 0.245 mole equal to 4.9 equivalents) is added. The evolving gas is led to an equipment for destruction (annihilation). The reaction mixture is kept in a bath of 50°-55° C. for 2.5 hours. Initially, the mixture becomes considerably thinner, then, in most cases, N-methyl-N'-{2-[(5-methylimidazol-4-yl)-methylthio]-ethyl}-N"-cyanoguanidine begins to precipitate without appearing of a complete solution. The mixture becomes thicker and eventually the stirring is stopped. After 2.5 hours the mixture is rapidly heated to 90° C. and stirred at this temperature for 30 minutes. The solution should not contain undissolved material. The solution is poured without cooling onto stirred ice (70 g). A clear solution of 0° to 10° C. is formed which becomes turbid and granular, and well-settling crystals separate. The solution is kept in a refrigerator for 2 hours, then filtered and washed with distilled water (2×10 ml). The wet weight of this precipitate is 14.8 g. After drying at 40° C., the dry weight of N-methyl-N'-{2-[(5-methylimidazol-4-yl)-methylthio]-ethyl}-N"-cyanoguanidine H is 12.27 g (90.82%); m.p. 73°-75° C.

後処理

  1. temperatureheated
  2. customThe evolving gas is led to an equipment for destruction (annihilation)
  3. customto precipitate
  4. stirringstirred at this temperature for 30 minutes
  5. additionThe solution is poured
  6. temperaturewithout cooling
  7. stirringonto stirred ice (70 g)
  8. customA clear solution of 0° to 10° C. is formed which
  9. customgranular, and well-settling crystals separate
  10. waitThe solution is kept in a refrigerator for 2 hours
  11. filtrationfiltered
  12. washwashed with distilled water (2×10 ml)
  13. customAfter drying at 40° C.

出典と根拠

ORDレコード
ord-7e9719e4367642ffba3f9370efb8cadc
出典データセット
uspto-grants-1986_04
特許番号
US04579954

反応ノート

読み込み中…