Trifluoroacetic acid → 5-(5h-Dibenzo[a,d]cyclohepten-5-yl)-2,4(1h,3h)-pyrimidinedione

HRID 1871964

반응식

HRID 1871964 반응식
CC(C)([O:4][C:5]1[N:10]=[C:9]([O:11]C(C)(C)C)[C:8]([C:16]2(O)[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[CH:20]=[CH:19][C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]2=3)=[CH:7][N:6]=1)C.C([SiH](CC)CC)C.FC(F)(F)C(O)=O>ClCCl>[CH:27]1[C:18]2[CH:19]=[CH:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[CH:16]([C:8]3[C:9](=[O:11])[NH:10][C:5](=[O:4])[NH:6][CH:7]=3)[C:17]=2[CH:30]=[CH:29][CH:28]=1

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 212508825-(2,4-bis(1,1-dimethylethoxy)pyrimidin-5-yl)-5H-dibenzo[a,d]cyclohepten-5-ol

생성물 1

HCID 110986755-(5h-Dibenzo[a,d]cyclohepten-5-yl)-2,4(1h,3h)-pyrimidinedione

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of the 5-(2,4-bis(1,1-dimethylethoxy)pyrimidin-5-yl)-5H-dibenzo[a,d]cyclohepten-5-ol and triethylsilane (64 ml) in dry dichloromethane (400 ml) at 0° C. was added trifluoroacetic acid (150 ml) dropwise over ten minutes. The cooling bath was removed and the solution was stirred at room temperature overnight. Toluene (300 ml) was added and solution was evaporated under vacuum. The residue was azeotroped with toluene (3 times). The oil was treated with diethyl ether and the precipitated product collected as a white powder (44 g).

후처리

  1. customThe cooling bath was removed
  2. additionToluene (300 ml) was added
  3. customsolution was evaporated under vacuum
  4. customThe residue was azeotroped with toluene (3 times)
  5. additionThe oil was treated with diethyl ether
  6. customthe precipitated product collected as a white powder (44 g)

출처 및 근거

ORD 기록
ord-f3e86daa6b7640d6946c5abe9950cbe6
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06107297

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