Methanol → 2-Thioadenosine

HRID 1729610

反応式

HRID 1729610 の反応式
C(O[N:4]=[C:5]([C:7]1[N:8]=[CH:9][N:10]([C@@H:13]2[O:19][C@H:18]([CH2:20][OH:21])[C@@H:16]([OH:17])[C@H:14]2[OH:15])[C:11]=1[NH2:12])[NH2:6])C.CO.[C:24](=S)=[S:25]>>[CH:9]1[N:10]([C@@H:13]2[O:19][C@H:18]([CH2:20][OH:21])[C@@H:16]([OH:17])[C@H:14]2[OH:15])[C:11]2[C:7](=[C:5]([NH2:6])[NH:4][C:24]([N:12]=2)=[S:25])[N:8]=1

参加物

4

反応物 3

HCID 887MethanolHCID 6348Carbon DisulfideHCID 53763093HCID 53763093、化合物

生成物 1

HCID 64519652-Thioadenosine

実験手順

0.45 g of 5-amino-1-β-D-ribofuranosylimidazole-4-carboxamide O-ethyl-oxime was dissolved in 8 ml of an aqueous solution containing 7 ml of methanol, and 2 ml of carbon disulfide was added to the solution. The resulting mixture was allowed to react in an autoclave at 120° C for 6 hours under autogenous pressure (about 10 Kg/cm2). The reaction mixture was concentrated to dryness, and the residue was dissolved in water. The aqueous solution was adjusted to a pH of 2 with hydrochloric acid, and the crystals thus precipitated were filtered to obtain 2-thioadenosine, which was then dissolved in aqueous ammonia, filtered and again adjusted to a pH of 2 with hydrochloric acid to obtain 0.355 g of pure 2-thioadenosine having a melting point of 199° C (with decomposition) in a 75% yield.

後処理

  1. additionwas added to the solution
  2. customto react in an autoclave at 120° C for 6 hours under autogenous pressure (about 10 Kg/cm2)
  3. concentrationThe reaction mixture was concentrated to dryness
  4. dissolutionthe residue was dissolved in water
  5. customthe crystals thus precipitated
  6. filtrationwere filtered

出典と根拠

ORDレコード
ord-75e78e4fc27e4e2cb3ac6078bb8e2e6a
出典データセット
uspto-grants-1976_11
特許番号
US03989682

関連ノート

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