Hydrochloric Acid → 3-(4-chloro-2-fluoro-5-isopropoxyphenyl)-1,5,6,7-tetrahydro-2H-cyclopenta[d]pyrimidine-2,4(3H)-dione

HRID 1722937노트

반응식

HRID 1722937 반응식
[Cl:1][C:2]1[C:7]([O:8][CH:9]([CH3:11])[CH3:10])=[CH:6][C:5]([NH:12][C:13](=[O:25])[NH:14][C:15]2[CH2:19][CH2:18][CH2:17][C:16]=2[C:20](OCC)=[O:21])=[C:4]([F:26])[CH:3]=1.C[O-].[Na+].Cl>CO>[Cl:1][C:2]1[C:7]([O:8][CH:9]([CH3:11])[CH3:10])=[CH:6][C:5]([N:12]2[C:20](=[O:21])[C:16]3[CH2:17][CH2:18][CH2:19][C:15]=3[NH:14][C:13]2=[O:25])=[C:4]([F:26])[CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 10942334Sodium MethoxideHCID 20026019HCID 20026019, 화합물

생성물 1

HCID 200260343-(4-chloro-2-fluoro-5-isopropoxyphenyl)-1,5,6,7-tetrahydro-2H-cyclopenta[d]pyrimidine-2,4(3H)-dione

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A suspension of 6.0 g of ethyl 2-[3-(4-chloro-2-fluoro-5-isopropoxyphenyl)ureido]-1-cyclopentenecarboxylate in 100 ml of absolute methanol is treated while stirring at room temperature with 7.8 ml of 2N sodium methylate solution and the reaction mixture is stirred for 2 hours. The solution is treated with 7.8 ml of 2N hydrochloric acid and evaporated to dryness. The residue is dissolved in 200 ml of ethyl acetate and the solution is washed with water, dried over anhydrous sodium sulphate and evaporated to dryness under reduced pressure. The residue is recrystallized from methylene chloride/diethyl ether. There is obtained 3-(4-chloro-2-fluoro-5-isopropoxyphenyl)-1,5,6,7-tetrahydro-2H-cyclopenta[d]pyrimidine-2,4(3H)-dione, m.p. 215°-217° C.

후처리

  1. additionis treated
  2. customevaporated to dryness
  3. dissolutionThe residue is dissolved in 200 ml of ethyl acetate
  4. washthe solution is washed with water
  5. dry with materialdried over anhydrous sodium sulphate
  6. customevaporated to dryness under reduced pressure
  7. customThe residue is recrystallized from methylene chloride/diethyl ether

출처 및 근거

ORD 기록
ord-b577cd24214e4fb2af649640b720ec14
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04859229

반응 노트

불러오는 중…