Acetic Acid → HCID 19911575、化合物

HRID 1533955ノート

反応式

HRID 1533955 の反応式
[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[CH2:7][NH:8]N1C=CC=CC1N.Cl.[Cl:17][CH2:18][C:19](=[NH:23])OCC.[C:24](O)(=O)[CH3:25]>>[Cl:17][CH2:18][C:19]1[N:8]([CH2:7][C:2]2[CH:3]=[N:4][CH:5]=[CH:6][N:1]=2)[C:2]2=[N:1][CH:6]=[CH:24][CH:25]=[C:3]2[N:23]=1

参加物

4

反応物 3

HCID 176Acetic AcidHCID 12470659Ethyl 2-chloroethanecarboximidate hydrochlorideHCID 67896527HCID 67896527、化合物

生成物 1

HCID 19911575HCID 19911575、化合物収率 100%

実験手順

To a stirred solution of 3.6 parts of N-(2-pyrazinylmethyl)-1,2-pyridinediamine in 30 parts of acetic acid were added 4.24 parts of ethyl 2-chloroethanimidate monohydrochloride. The reaction mixture was stirred first for 21 hours at room temperature and then for a few minutes at 90° C. The whole was evaporated and the residue was taken up in water. The aqueous layer was treated with sodium carbonate and the product was extracted with dichloromethane. The extract was dried, filtered and evaporated, yielding 3.9 parts (100%) of 2-(chloromethyl)-3-(2-pyrazinylmethyl)-3H-imidazo[4,5-b]pyridine as a residue (int. 29).

後処理

  1. waitfor a few minutes at 90° C
  2. customThe whole was evaporated
  3. additionThe aqueous layer was treated with sodium carbonate
  4. extractionthe product was extracted with dichloromethane
  5. customThe extract was dried
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-db1a2b3cdfc447ed95fc7ac4025f816a
出典データセット
uspto-grants-1992_02
特許番号
US05086056

反応ノート

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