Chloroacetic Acid → 5,6-Dimethyluracil

HRID 63094

反応式

HRID 63094 の反応式
[CH3:1][C:2]1[C:3](=[O:10])[NH:4][C:5](=S)[NH:6][C:7]=1[CH3:8].ClCC(O)=[O:14]>O>[CH3:1][C:2]1[C:3](=[O:10])[NH:4][C:5](=[O:14])[NH:6][C:7]=1[CH3:8]

参加物

4

反応物 2

HCID 300Chloroacetic AcidHCID 27362495,6-Dimethyl-2-thiouracil

生成物 1

HCID 960315,6-Dimethyluracil収率 81.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 5,6-dimethyl-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (14.4 g, 0.09 mol, Step A) and chloroacetic acid (100.0 g, 1.06 mol) in water (43 mL) was refluxed overnight, cooled down to ambient temperature and quenched with water (500 mL). The formed precipitate was collected by filtration and dried to yield 10.3 g (79.7%) of the titled compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.70 (s, 3H) 2.02 (s, 3H) 10.56 (s, 1H) 10.86 (s, 1H).

後処理

  1. customquenched with water (500 mL)
  2. filtrationThe formed precipitate was collected by filtration
  3. customdried

出典と根拠

ORDレコード
ord-1cf59a9992694d7bb67f93f1ff275d11
出典データセット
uspto-grants-2016_09
特許番号
US09447051B2

関連ノート

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