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Ammonia → HCID 67164793, 화합물

HRID 552751
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HRID 552751 반응식
[NH2:1][C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[C@H:11]1[C@@H:15]2[O:16][C:17]([CH3:20])([CH3:19])[O:18][C@@H:14]2[C@@H:13]([CH2:21][OH:22])[O:12]1.C[Si](Cl)(C)C.[Br:28][C:29]1[CH:37]=[CH:36][C:32]([C:33](Cl)=[O:34])=[CH:31][CH:30]=1.N>N1C=CC=CC=1.O>[Br:28][C:29]1[CH:37]=[CH:36][C:32]([C:33]([NH:1][C:2]2[N:10]=[CH:9][N:8]=[C:7]3[C:3]=2[N:4]=[CH:5][N:6]3[C@H:11]2[C@H:15]3[C@H:14]([O:18][C:17]([CH3:19])([CH3:20])[O:16]3)[C@@H:13]([CH2:21][OH:22])[O:12]2)=[O:34])=[CH:31][CH:30]=1
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참가 물질

7

반응물 4

HCID 222AmmoniaHCID 6397ChlorotrimethylsilaneHCID 685154-Bromobenzoyl chlorideHCID 2723654((3aR,4R,6R,6aR)-6-(6-Amino-9H-purin-9-yl)-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxol-4-yl)methanol

생성물 1

HCID 67164793HCID 67164793, 화합물수율 49%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 1049Pyridine용매2회

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온도
0 °C

실험 절차

[(3aR,4R,6R,6aR)-6-(6-amino-9H-purin-9-yl)-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxol-4-yl]methanol (0.400 g, 1.30 mmol) was dried by co-evaporation with pyridine, then suspended in dry pyridine (6.5 mL). TMSCl (0.330 mL, 2.60 mmol) was added and the mixture was stirred for 15 min. 4-Bromobenzoylchloride (0.342 g, 1.56 mmol) was added to the mixture and stirred for 2 h. The solution was cooled to 0° C. and 1 mL of H2O was added. After 5 min a 29% NH3 aq solution (0.847 mL) was added and the reaction mixture was stirred for 30 min while warming to r.t. The mixture was then concentrated and the residue was diluted with H2O (40 mL). The product was extracted with EtOAc (60 mL) and concentrated. The crude material was purified by flash chromatography (65 to 100% EtOAc/hexanes) to afford the title compound (0.305 g, 49%).

후처리

  1. stirringstirred for 2 h
  2. stirringthe reaction mixture was stirred for 30 min
  3. temperaturewhile warming to r.t
  4. concentrationThe mixture was then concentrated
  5. additionthe residue was diluted with H2O (40 mL)
  6. extractionThe product was extracted with EtOAc (60 mL)
  7. concentrationconcentrated
  8. customThe crude material was purified by flash chromatography (65 to 100% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-bb4517ba29a748ebb3d3a55c4b8145aa
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07951810B2

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