Pyridine → HCID 178522340、化合物

HRID 1735952ノート

反応式

HRID 1735952 の反応式
[CH2:1]([O:8][C:9](Cl)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClC(N[N:16]1[CH:24]=[C:22](C)[C:20](=O)[NH:19][C:17]1=[O:18])=O.[N:25]1C=CC=CC=1>>[CH2:1]([O:8][C:9]([NH:25][C:20]1[CH:22]=[CH:24][NH:16][C:17](=[O:18])[N:19]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 3

HCID 1049PyridineHCID 10387Benzyl chloroformateHCID 19076265HCID 19076265、化合物

生成物 1

HCID 178522340HCID 178522340、化合物

反応条件

温度
0 °C

実験手順

Over a period of about 1 h, benzyloxycarbonyl chloride (52 ml; 0.36 mol) was added dropwise to a suspension of cytosine (8, 20.0 g; 0.18 mol) in dry pyridine (1000 ml) at 0° C. under nitrogen in oven-dried equipment. The solution then was stirred overnight, after which the pyridine suspension was evaporated to dryness, in vacuo. Water (200 ml) and 4N hydrochloric acid were added to reach pH~1. The resulting white precipitate was filtered off, washed with water and partially dried by air suction. The still-wet precipitate was boiled with absolute ethanol (500 ml) for 10 min, cooled to 0° C., filtered, washed thoroughly with ether, and dried, in vacuo. Yield 24.7 g (54%). M.p.>250° C. Anal. for C12H11N3O3. Found (calc.); C: 58.59(58.77); H: 4.55(4.52); N: 17.17(17.13). No NMR spectra were recorded since it was not possible to get the product dissolved.

後処理

  1. customafter which the pyridine suspension was evaporated to dryness, in vacuo
  2. additionWater (200 ml) and 4N hydrochloric acid were added
  3. filtrationThe resulting white precipitate was filtered off
  4. washwashed with water
  5. custompartially dried by air suction
  6. waitThe still-wet precipitate was boiled with absolute ethanol (500 ml) for 10 min
  7. filtrationfiltered
  8. washwashed thoroughly with ether
  9. customdried, in vacuo
  10. customto get the product
  11. dissolutiondissolved

出典と根拠

ORDレコード
ord-09ecc43c3f1649fb90123f272f8df593
出典データセット
uspto-grants-1996_07
特許番号
US05539082

反応ノート

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