Diethyl Ether → 5,6-Diphenyl-1-methyl-2(1H)-pyrimidinone

HRID 12570

반응식

HRID 12570 반응식
O/[C:2](/[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[C:3](/[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)\[CH:4]=O.CC1C=CC(S(O)(=O)=O)=CC=1.[CH3:29][NH:30][C:31]([NH2:33])=[O:32].C(OCC)C>C1(C)C=CC=CC=1.C(Cl)Cl>[CH3:29][N:30]1[C:2]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:3]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[CH:4]=[N:33][C:31]1=[O:32]

참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 6101p-Toluenesulfonic acidHCID 11719MethylureaHCID 178520855HCID 178520855, 화합물

생성물 1

HCID 36093525,6-Diphenyl-1-methyl-2(1H)-pyrimidinone

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매

실험 절차

A solution of (Z)-3-hydroxy-2,3-diphenyl-propenal (105, 423 mg, 1.89 mmol), pTSA (30 mg, 7.56 mmol) and methyl urea (118 mg, 0.62 mmol) in toluene was heated at 110° C. overnight. The reaction was quenched with water, and the products were extracted with ethyl acetate. The organic layer was separated and washed with brine, and dried over MgSO4, and concentrated in vacuo to produce a yellow oil. The crude product was dissolved in CH2Cl2 and titrated with diethyl ether to give the title compound as a white solid.

후처리

  1. customThe reaction was quenched with water
  2. extractionthe products were extracted with ethyl acetate
  3. customThe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. customto produce a yellow oil

출처 및 근거

ORD 기록
ord-14f27c1bba5a4c2dbfbfd7cb6108016d
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728014B2

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