N-Methyl-2,2'-diaminodiethylamine → HCID 22152287、化合物

HRID 1111329ノート

反応式

HRID 1111329 の反応式
[NH2:1][CH2:2][CH2:3][N:4]([CH3:8])[CH2:5][CH2:6][NH2:7].[NH2:9][C:10]1[C:11]([C:18](N2C=CN=C2)=[O:19])=[N:12][C:13]([Cl:17])=[C:14]([NH2:16])[N:15]=1>O1CCCC1>[NH2:9][C:10]1[C:11]([C:18]([NH:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][NH2:7])[CH3:8])=[O:19])=[N:12][C:13]([Cl:17])=[C:14]([NH2:16])[N:15]=1

参加物

4

反応物 2

HCID 430288N-Methyl-2,2'-diaminodiethylamineHCID 13020010(3,5-diamino-6-chloropyrazin-2-yl)(1H-imidazol-1-yl)methanone

生成物 1

HCID 22152287HCID 22152287、化合物収率 69,354.797%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 84.0 g (0.744 mol) of N-(2-aminoethyl)-N-methyl-1,2-ethanediamine (see U.S. Pat. No. 3,201,472 for a method of obtaining this compound) in 700 ml of tetrahydrofuran was added 88.6 g (0.372 mmol) of 1-(3,5-diamino-6-chloropyrazinoyl)imidazole in 10 portions over 1 5 h. After 1 h at ambient temperature the reaction mixture was filtered and concentrated to 300 ml. The solution was added dropwise to 1.4 liters of ether with vigorous stirring. The solid was filtered, washed with ether and dried. There was obtained 74.3 g (0.258 mol, 70%) of 3,5-diamino-N-[2-[(2-aminoethyl)methylamino]ethyl]-6chloropyrazinecarboxamide. A sample was filtered through a pad of silica gel and eluted with 5:95 (v/v) methanol:methylene chloride saturated with ammonia gas mp 138°-139.5° C.

後処理

  1. filtrationAfter 1 h at ambient temperature the reaction mixture was filtered
  2. concentrationconcentrated to 300 ml
  3. additionThe solution was added dropwise to 1.4 liters of ether with vigorous stirring
  4. filtrationThe solid was filtered
  5. washwashed with ether
  6. customdried

出典と根拠

ORDレコード
ord-08ea98766d7844d98b7ac2d8ac30bbb8
出典データセット
uspto-grants-1990_12
特許番号
US04980352

反応ノート

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