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Potassium Carbonate → 1-(2-Hydroxy-3,3,3-trichloropropyl)-5-bromopyrimid-2-one

HRID 1075145
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HRID 1075145 반응식
[Br:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[NH:6][CH:7]=1.[O:9]1[CH:11]([C:12]([Cl:15])([Cl:14])[Cl:13])[CH2:10]1.C([O-])([O-])=O.[K+].[K+]>CN(C)C=O>[OH:9][CH:11]([C:12]([Cl:15])([Cl:14])[Cl:13])[CH2:10][N:4]1[CH:3]=[C:2]([Br:1])[CH:7]=[N:6][C:5]1=[O:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 183212-(Trichloromethyl)oxiraneHCID 1014945-Bromo-2(1H)-pyrimidinone

생성물 1

HCID 204943081-(2-Hydroxy-3,3,3-trichloropropyl)-5-bromopyrimid-2-one수율 52%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A stirred mixture of 5-bromopyrimid-2-one (0.009 mol), 1,2-epoxy-3,3,3-trichloropropane (0.009 mol) and K2CO3 (33 mg) in dimethylformamide (40 ml ) was heated at 80° C. for 4 h. The reaction mixture was then evaporated to dryness at reduced pressure (1 mm Hg). The crystalline residue was triturated with a little ether and dissolved in ethyl acetate. The filtered ethyl acetate solution was concentrated to about 50 ml and left in the cold when the product crystallized out in 52% yield. m.p. 210°-212° C. (ethyl acetate).

후처리

  1. customThe reaction mixture was then evaporated to dryness at reduced pressure (1 mm Hg)
  2. customThe crystalline residue was triturated with a little ether
  3. dissolutiondissolved in ethyl acetate
  4. concentrationThe filtered ethyl acetate solution was concentrated to about 50 ml
  5. waitleft in the cold when the product
  6. customcrystallized out in 52% yield

출처 및 근거

ORD 기록
ord-81e1ed89da8d4ea4881280598e77f346
출처 데이터셋
uspto-grants-1983_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04395406

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