Trifluoroacetic acid → HCID 178419102, 화합물

HRID 10466

반응식

HRID 10466 반응식
[C:1]1([CH:7]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:8][NH:9][C:10]2[N:18]=[C:17]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][N:14]3C2CCCCO2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.FC(F)(F)C(O)=O>C(O)C>[C:30]1([CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:8][NH:9][C:10]2[N:18]=[C:17]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][NH:14]3)[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 21978293Ethyl 6-[(2,2-diphenylethyl)amino]-9-(tetrahydro-2H-pyran-2-yl)-9H-purine-2-carboxylate

생성물 1

HCID 178419102HCID 178419102, 화합물수율 100.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of ethyl 6-[(2,2-diphenylethyl)amino]-9-(tetrahydro-2H-pyran-2-yl)-9H-purine-2-carboxylate (Preparation 62) (250 g, 0.530 moles) in absolute ethanol (1250 ml) under an atmosphere of nitrogen was added trifluoroacetic acid (73.5 g, 0.645 moles) and the resultant mixture was heated at 50° C. for 20 hours. The mixture was cooled and the solid was collected by filtration. The filter cake was washed with absolute ethanol (350 ml) and was then dried in vacuo at 50° C. to give the title compound (206.5 g) as a cream coloured fine powder, m.p. >200° C.

후처리

  1. temperatureThe mixture was cooled
  2. filtrationthe solid was collected by filtration
  3. washThe filter cake was washed with absolute ethanol (350 ml)
  4. customwas then dried in vacuo at 50° C.

출처 및 근거

ORD 기록
ord-81c01a4908cd47028c7b6659b5d734b4
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094769B2

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