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Ammonia → N2 (phenylacetyl)-guanosine

HRID 54641
ノート
印刷プレビュー

反応式

HRID 54641 の反応式
[C@@H:1]1([N:10]2[C:20]3[N:19]=[C:17]([NH2:18])[NH:16][C:14](=[O:15])[C:13]=3[N:12]=[CH:11]2)[O:9][C@H:6]([CH2:7][OH:8])[C@@H:4]([OH:5])[C@H:2]1[OH:3].C[Si](Cl)(C)C.[C:26]1([CH2:32][C:33](Cl)=[O:34])[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.[NH3:36].[K+].[Br-]>N1C=CC=CC=1.CCO.O>[N:36]#[N:10].[C:26]1([CH2:32][C:33]([C@@:1]2([N:10]3[C:20]4[N:19]=[C:17]([NH2:18])[NH:16][C:14](=[O:15])[C:13]=4[N:12]=[CH:11]3)[O:9][C@H:6]([CH2:7][OH:8])[C@@H:4]([OH:5])[C@H:2]2[OH:3])=[O:34])[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 222AmmoniaHCID 6397ChlorotrimethylsilaneHCID 7679Phenylacetyl chlorideHCID 253877Potassium BromideHCID 135398635Guanosine

生成物 1

HCID 136381147N2 (phenylacetyl)-guanosine収率 59%

試薬・触媒・溶媒 3

HCID 702
Ethanol
溶媒
HCID 962Water溶媒
HCID 1049Pyridine溶媒2 回

実験手順

Guanosine 5 (10.19 g, 36 mmoles) was dried three times by coevaporation with dry pyridine and suspended in 200 ml of dry pyridine. To this was added trimethylsilyl chloride (24 ml, 180 mmoles) at room temperature. After the solution was stirred for 1 hour at room temperature, phenylacetyl chloride (24 ml, 180 mmoles) was added dropwise and the solution was maintained at room temperature with mechanical stirring for 15 hours. The reaction mixture was cooled in an ice bath, and 75 ml of cold water added. After 30 minutes, 75 ml of 29% aqueous ammonia was added and the reaction mixture was stirred for 30 minutes. The solution was then evaporated to near dryness, and the residue was dissolved in 300 ml water and 300 ml methylene chloride. The product crystallizing out of the aqueous solution upon extraction with CH2Cl2 was filtered off, washed with CH2Cl2 (3×70 ml) and ether (3×70 ml) and air dried to yield 8.5 g (59% yield) of Ribo GPA 6. The product was characterized as follows: m.p. 160°-170° C. (dec.); UV (EtOH): λ max 280 nm and 258 nm; IR (KBr): ν 1680 (vs, C=O of amide), 1722 (s, C=O of amide ring), and 3000-3500 (NHOH) cm-1 ; 1H-NMR (DMSO-d6): δ 3.53 and 3.57 (2m, 2H, C5, CH2), 3.81 (s, 2H, C6H5CH2), 3.91 (d, 1H, C4'H), 4.13 (m, 1H, C3' H), 4.42 (d, 1H, C2' H), 5.08 (br, s, 1H, C5' OH), 5.21 (br, s, 1H, C3' OH), 5.81 (d, 1H, J1',2' =5.64 Hz, C1' H), 7.26-7.41 (m, 5H, C6H5), 8.28 (s, 1H, C8H), 11.99 and 12.01 (2s, 2H, 2×NHCO). Calcd for C18H19N5O6 (401.37): C, 53.86; H, 4.77; N, 17.45. Found: C, 53.49; H, 5.11; N, 17.36

後処理

  1. temperaturethe solution was maintained at room temperature
  2. stirringwith mechanical stirring for 15 hours
  3. temperatureThe reaction mixture was cooled in an ice bath
  4. waitAfter 30 minutes
  5. stirringthe reaction mixture was stirred for 30 minutes
  6. customThe solution was then evaporated
  7. dissolutionthe residue was dissolved in 300 ml water
  8. customThe product crystallizing out of the aqueous solution upon extraction with CH2Cl2
  9. filtrationwas filtered off
  10. washwashed with CH2Cl2 (3×70 ml) and ether (3×70 ml) and air
  11. customdried
  12. customto yield 8.5 g (59% yield) of Ribo GPA 6

出典と根拠

ORDレコード
ord-e367d03f3de449a78c7cdb41e874be5b
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05623068

反応ノート

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