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2,4,6-Trichloropyrimidine → HCID 19428516, 화합물

HRID 1721297
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HRID 1721297 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]([CH3:15])([CH3:14])[CH3:13]>O1CCCC1>[Cl:9][C:4]1[CH:5]=[C:6]([Cl:8])[N:7]=[C:2]([NH:10][CH2:11][C:12]([CH3:15])([CH3:14])[CH3:13])[N:3]=1
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참가 물질

4

반응물 2

HCID 773782,4,6-TrichloropyrimidineHCID 79882Neopentylamine

생성물 1

HCID 19428516HCID 19428516, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

25 g (136.3 mmoles) of 2,4,6-trichloropyrimidine are dropwise added to a mixture of 23.84 g (273.5 mmoles) of 1-amino-2,2-dimethylpropane and 200 ml of tetrahydrofuran at a temperature between 10° C. and 15° C. while stirring and cooling. Thereafter, the reaction mixture is stirred at room temperature for an additional 30 minutes, then evaporated. After distributing the evaporation residue between 300 ml of chloroform and 50 ml of 10% sodium hydroxide solution, the organic phase is separated, washed 4 times with 100 ml of water each, then dried and evaporated. The evaporation residue is subjected to chromatography on a silica gel column. By using a 19:1 mixture of hexane and ethyl acetate, 4,6-dichloro-2-(2,2-dimethylpropylamino)pyrimidine is obtained, which is recrystallized from a mixture of ether and hexane to obtain a yield of 13.60 g (42.6%), m.p.: 63°-66° C.

후처리

  1. temperaturecooling
  2. stirringThereafter, the reaction mixture is stirred at room temperature for an additional 30 minutes
  3. customevaporated
  4. customthe organic phase is separated
  5. washwashed 4 times with 100 ml of water each,
  6. customthen dried
  7. customevaporated
  8. additiona 19:1 mixture of hexane and ethyl acetate

출처 및 근거

ORD 기록
ord-f44c43a42904454388914e3ab44a822f
출처 데이터셋
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05510345

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