Dimethylformamide → (1-(7-Benzyl-1,3-dimethyl-2,6-dioxo-1,2,3,6-tetrahydropurin-8-yl)pyrrolidin-3-yl)carbamic acid tert-butyl ester

HRID 458618

반응식

HRID 458618 반응식
[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH3:18])[C:13](=[O:19])[N:12]([CH3:20])[C:11]=2[N:10]=[C:9]1Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:22]([O:26][C:27]([NH:29][C@H:30]1[CH2:34][CH2:33][NH:32][CH2:31]1)=[O:28])([CH3:25])([CH3:24])[CH3:23].C(N(CC)CC)C.CN(C=O)C>CC(O)C>[C:22]([O:26][C:27](=[O:28])[NH:29][CH:30]1[CH2:34][CH2:33][N:32]([C:9]2[N:8]([CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:16]3[C:15](=[O:17])[N:14]([CH3:18])[C:13](=[O:19])[N:12]([CH3:20])[C:11]=3[N:10]=2)[CH2:31]1)([CH3:25])([CH3:23])[CH3:24]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 3253727-Benzyl-8-chloro-1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dioneHCID 1514396(3S)-(-)-3-(tert-Butoxycarbonylamino)pyrrolidine

생성물 1

HCID 69136344(1-(7-Benzyl-1,3-dimethyl-2,6-dioxo-1,2,3,6-tetrahydropurin-8-yl)pyrrolidin-3-yl)carbamic acid tert-butyl ester

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

7-Benzyl-8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione (2A) (100 mg, 0.33 mmol), (3S)-(−)-3-(tert-butoxycarbonylamino)pyrrolidine (305 mg, 1.64 mmol), and triethylamine (0.46 ml, 3.28 mmol) was dissolved in 20 ml of 2-propanol and 5 ml of DMF and the mixture was subjected to microwaves (method F, 130° C., 300 W) for three hours. The solvent was evaporated and the crude product was purified by preparative HPLC (method A1, Rt=11.75 min.). Evaporation of the solvent afforded compound (3A) as a brown oil.

후처리

  1. customThe solvent was evaporated
  2. customthe crude product was purified by preparative HPLC (method A1, Rt=11.75 min.)
  3. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-ab4c48330f244552b739e231d2105881
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192952B2

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