Sodium Carbonate → 5-Chloro-1-(3-thienylmethyl)pyrimidin-2-one

HRID 434643

反応式

HRID 434643 の反応式
Cl.[Cl:2][C:3]1[CH:4]=[N:5][C:6](=[O:9])[NH:7][CH:8]=1.Br[CH2:11][C:12]1[CH:16]=[CH:15][S:14][CH:13]=1.C(=O)([O-])[O-].[Na+].[Na+]>[Cl-].C([N+](C)(C)C)C1C=CC=CC=1.CN(C)C=O.O>[Cl:2][C:3]1[CH:4]=[N:5][C:6](=[O:9])[N:7]([CH2:11][C:12]2[CH:16]=[CH:15][S:14][CH:13]=2)[CH:8]=1

参加物

7

反応物 3

HCID 10340Sodium CarbonateHCID 5207033-(Bromomethyl)thiopheneHCID 126485235-Chloropyrimidin-2-ol hydrochloride

生成物 1

HCID 204917595-Chloro-1-(3-thienylmethyl)pyrimidin-2-one収率 34.2%

試薬・触媒・溶媒 3

HCID 5963Benzyltrimethylammonium chloride触媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 5-chloropyrimidin-2-one hydrochloride (502 mg), 3-bromomethylthiophene (1.069 g), anhydrous sodium carbonate (955 mg) and benzyltrimethylammonium chloride (12 mg) in dry N,N-dimethylformamide (15 ml) was stirred at room temperature. After 22 h the reaction mixture was diluted with water (120 ml) and the resulting precipitate was collected, washed with water and dried to give a pale yellow solid (233 mg). The solid was crystallised from ethanol to give white crystals of the title thiophene (184 mg), m.p. 194°-195° C., λmax 229 nm (ε 14,410), 233 nm (ε 3,080), λinf 246 nm (ε 5,210).

後処理

  1. customthe resulting precipitate was collected
  2. washwashed with water
  3. customdried

出典と根拠

ORDレコード
ord-2b8a98689de64f6a9cfeb696e26be292
出典データセット
uspto-grants-1983_08
特許番号
US04399140

関連ノート

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