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Hydrochloric Acid → 3-Pentyl-2-thioxo-1,2,3,7-tetrahydro-6H-purin-6-one

HRID 1787750
ノート
印刷プレビュー

反応式

HRID 1787750 の反応式
C(N[C:10]([N:12]([CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[C:13]1[N:14]=[CH:15][NH:16][C:17]=1[C:18]([NH2:20])=[O:19])=[S:11])(=O)C1C=CC=CC=1.[OH-].[Na+].Cl>O>[CH2:21]([N:12]1[C:13]2[N:14]=[CH:15][NH:16][C:17]=2[C:18](=[O:19])[NH:20][C:10]1=[S:11])[CH2:22][CH2:23][CH2:24][CH3:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 576001664-[[(Benzoylamino)carbonothioyl](pentyl)amino]-1H-imidazole-5-carboxamide

生成物 1

HCID 576002363-Pentyl-2-thioxo-1,2,3,7-tetrahydro-6H-purin-6-one収率 94%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 4-[[(benzoylamino)carbonothioyl](pentyl)amino]-1H-imidazole-5-carboxamide (11.8 g, 0.0263 mol) and 1 M of sodium hydroxide in water (75 mL) was heated to reflux for 3 h. Solid was formed in the reaction mixture. The reaction mixture was adjusted to pH 3-4 with concentrated HCl with cooling in an ice bath. The solid was filtered, washed with water and air-dried to give the product (9.0 g, 65% purity, 94% yield). The product was used for the next step without further purification. LCMS calculated for C10H15N4OS (M+H): 239.1; found: 239.1.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 3 h
  3. customSolid was formed in the reaction mixture
  4. temperaturewith cooling in an ice bath
  5. filtrationThe solid was filtered
  6. washwashed with water
  7. customair-dried
  8. customto give the product (9.0 g, 65% purity, 94% yield)
  9. customThe product was used for the next step without further purification

出典と根拠

ORDレコード
ord-c4e9d8453a0f47fab13d4cea37fbad55
出典データセット
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07511050B2

反応ノート

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