1,2-Hydrazinedicarboxamide → 1-(3,5-Dioxo-1,2,4-triazolidin-4-yl-methyl)-1,3,3-trimethyl-5-(3,5-dioxo-1,2,4-triazolidin-4-yl)-cyclohexane

HRID 851793

反応式

HRID 851793 の反応式
[NH2:1][CH2:2][C:3]1([CH3:12])[CH2:8][CH:7]([NH2:9])[CH2:6][C:5]([CH3:11])([CH3:10])[CH2:4]1.[C:13]([NH:16][NH:17][C:18](N)=[O:19])(N)=[O:14]>CN1CCCC1=O>[O:14]=[C:13]1[N:1]([CH2:2][C:3]2([CH3:12])[CH2:8][CH:7]([N:9]3[C:18](=[O:19])[NH:17][NH:16][C:13]3=[O:14])[CH2:6][C:5]([CH3:11])([CH3:10])[CH2:4]2)[C:18](=[O:19])[NH:17][NH:16]1

参加物

4

反応物 2

HCID 80391,2-HydrazinedicarboxamideHCID 17857Isophorone diamine

生成物 1

HCID 205012001-(3,5-Dioxo-1,2,4-triazolidin-4-yl-methyl)-1,3,3-trimethyl-5-(3,5-dioxo-1,2,4-triazolidin-4-yl)-cyclohexane

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

765 g of 1-aminomethyl-5-amino-1,3,3-trimethyl cyclohexane and 708 g of hydrazodicarbonamide are stirred in 1 liter of N-methyl pyrrolidone for 4 hours at 175° C., for 5 hours at 200° C. and for 15 hours at 220° C. The solvent is then distilled off in vacuo and the residue is dried in vacuo, giving 1473 g (97% of the theoretical) of 1-(3,5-dioxo-1,2,4-triazolidin-4-yl-methyl)-1,3,3-trimethyl-5-(3,5-dioxo-1,2,4-triazolidin-4-yl)-cyclohexane in the form of colourless crystals melting at 213 C. (decomposition).

後処理

  1. distillationThe solvent is then distilled off in vacuo
  2. customthe residue is dried in vacuo

出典と根拠

ORDレコード
ord-49e66688c7f741a58513d0d398a2048b
出典データセット
uspto-grants-1983_05
特許番号
US04386213

関連ノート

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