Pyridine → HCID 178464036, 화합물

HRID 1390016

반응식

HRID 1390016 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 178464036HCID 178464036, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-2ff7e962a7bd4016a3920dcb75a0c7cb
출처 데이터셋
uspto-grants-1981_01
특허 번호
US04247556

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