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2,4,6-Trichloropyrimidine → HCID 19428495, 화합물

HRID 1078955
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HRID 1078955 반응식
Cl[C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.[NH2:10][CH2:11][C:12]([CH3:17])([CH3:16])[CH2:13][CH:14]=[CH2:15]>O1CCCC1>[Cl:9][C:4]1[CH:5]=[C:6]([Cl:8])[N:7]=[C:2]([NH:10][CH2:11][C:12]([CH3:17])([CH3:16])[CH2:13][CH:14]=[CH2:15])[N:3]=1
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참가 물질

4

반응물 2

HCID 773782,4,6-TrichloropyrimidineHCID 6418312,2-Dimethylpent-4-en-1-amine

생성물 1

HCID 19428495HCID 19428495, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

4.59 (25 mmoles) of 2,4,6-trichloropyrimidine are added to a solution of 6.23 g (55 mmoles) of 5-amino-4,4-dimethyl-1-pentene in 50 ml of tetrahydrofuran at room temperature, the reaction mixture is stirred at the same temperature for 4 hours, then evaporated. The evaporation residue is distributed between 60 ml of chloroform and 5 ml of 10% sodium hydroxide solution. After separation the organic phase is washed 4 times with 10 ml of water each, then dried and evaporated. The evaporation residue is subjected to chromatography on a silica gel column by using mixtures of hexane and ethyl acetate as eluents. Elution with a 19:1 hexane/ethyl acetate mixture gives 4,6-dichloro-2-[(2,2-dimethyl-4-penten-1-yl)amino]pyrimidine as an oily product in a yield of 2.62 g (40.3%).

후처리

  1. customevaporated
  2. customAfter separation the organic phase
  3. washis washed 4 times with 10 ml of water each,
  4. customthen dried
  5. customevaporated
  6. washElution with a 19:1 hexane/ethyl acetate mixture

출처 및 근거

ORD 기록
ord-c6d53bcacb0b486795e4a3ae6d1a2500
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05550240

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