Triethylamine → HCID 12671194、化合物

HRID 435976ノート

反応式

HRID 435976 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 12671194HCID 12671194、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-ef398a7d0cf74e24860472c66a5b7f2e
出典データセット
uspto-grants-1977_02
特許番号
US04007189

反応ノート

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