Pyridine → HCID 178464036、化合物

HRID 1390016

反応式

HRID 1390016 の反応式
[CH2:1]([N:3]([CH2:15][CH3:16])[CH2:4][CH2:5][NH:6][C:7]1[C:12]([NH2:13])=[CH:11][CH:10]=[C:9]([Cl:14])[N:8]=1)[CH3:2].N1C=CC=CC=1.Cl[C:24](OCC)=[O:25]>O1CCOCC1>[CH2:15]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][N:6]1[C:7]2[N:8]=[C:9]([Cl:14])[CH:10]=[CH:11][C:12]=2[N:13]=[C:24]1[OH:25])[CH3:16]

参加物

5

反応物 3

HCID 1049PyridineHCID 10928Ethyl chloroformateHCID 202947442-(2-Diethylaminoethylamino)-3-amino-6-chloropyridine

生成物 1

HCID 178464036HCID 178464036、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

The solution of 80 grams of 2-(2-diethylaminoethylamino)-3-amino-6-chloropyridine in 900 ml of dioxane was treated with stirring with 32 ml of pyridine and 36.6 ml of ethyl chloroformate and stirred for one hour. The product precipitating thereby was washed with water and dried (2-(2-diethylaminoethylamino)-3-carbethoxy-amino-6-chloropyridine, M.P. 205°-206° C.) and subsequently melted with occasional stirring and held for 3 hours at 190°-210° C. After cooling the solidified melt was recrystallized from methanol under the addition of activated carbon and isopropanolic H Cl. M.P. of the hydrochloride 252°-254° C.; Yield 52.8 grams.

後処理

  1. customThe product precipitating
  2. washthereby was washed with water
  3. dry with materialdried (2-(2-diethylaminoethylamino)-3-carbethoxy-amino-6-chloropyridine, M.P. 205°-206° C.)
  4. stirringwith occasional stirring
  5. waitheld for 3 hours at 190°-210° C
  6. temperatureAfter cooling the solidified melt
  7. customwas recrystallized from methanol under the addition of activated carbon and isopropanolic H Cl
  8. customM.P. of the hydrochloride 252°-254° C.

出典と根拠

ORDレコード
ord-2ff7e962a7bd4016a3920dcb75a0c7cb
出典データセット
uspto-grants-1981_01
特許番号
US04247556

関連ノート

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