N-Methyl-2,2'-diaminodiethylamine → HCID 22152287, 화합물

HRID 1111329노트

반응식

HRID 1111329 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 22152287HCID 22152287, 화합물수율 69,354.797%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-08ea98766d7844d98b7ac2d8ac30bbb8
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04980352

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