Triethylamine → HCID 12671194, 화합물

HRID 435976노트

반응식

HRID 435976 반응식
Cl[C:2]1[N:7]2[N:8]=[CH:9][N:10]=[C:6]2[N:5]=[C:4]([CH3:11])[C:3]=1[CH2:12][CH2:13]Cl.Cl.[CH2:16]([NH2:20])[CH2:17][CH2:18][CH3:19].C(N(CC)CC)C>C(O)C>[CH2:16]([N:20]1[C:2]2[N:7]3[N:8]=[CH:9][N:10]=[C:6]3[N:5]=[C:4]([CH3:11])[C:3]=2[CH2:12][CH2:13]1)[CH2:17][CH2:18][CH3:19]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 36386487-chloro-6-(2-chloroethyl)-5-methyl[1,2,4]triazolo[1,5-a]pyrimidineHCID 64324001-Butanamine, hydrochloride (1:1)

생성물 1

HCID 12671194HCID 12671194, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 2g of 7-chloro-6-(2-chloroethyl)-5-methyl-s-triazolo[1,5-a]pyrimidine, 0.95g of n-butylamine hydrochloride, 4 ml of triethylamine and 20 ml of ethanol was stirred under reflux for 1 hour. The reaction mixture was then concentrated under reduced pressure and the residue was dissolved in chloroform and purified by an column chromatography of alumina. The crystals thus obtained were recrystallized from isopropyl ether affording 1.35g of pale yellow needles of m.p. 72° - 75° C.

후처리

  1. temperatureunder reflux for 1 hour
  2. concentrationThe reaction mixture was then concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in chloroform
  4. custompurified by an column chromatography of alumina
  5. customThe crystals thus obtained
  6. customwere recrystallized from isopropyl ether affording 1.35g of pale yellow needles of m.p. 72° - 75° C.

출처 및 근거

ORD 기록
ord-ef398a7d0cf74e24860472c66a5b7f2e
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04007189

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