Boron tribromide → HCID 178503544、化合物

HRID 705979ノート

反応式

HRID 705979 の反応式
C[O:2][C:3]1[N:8]=[CH:7][C:6]([CH2:9][C:10]2[C:11](=[O:18])[N:12]=[C:13]([S:16][CH3:17])[NH:14][CH:15]=2)=[CH:5][N:4]=1.B(Br)(Br)Br>O>[CH3:17][S:16][C:13]1[NH:14][CH:15]=[C:10]([CH2:9][C:6]2[CH:5]=[N:4][C:3](=[O:2])[NH:8][CH:7]=2)[C:11](=[O:18])[N:12]=1

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 178494160HCID 178494160、化合物

生成物 1

HCID 178503544HCID 178503544、化合物収率 26.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

Entire reaction was performed under argon atmosphere using syringe septa technique. 5-(2-methoxy-pyrimidin-5-ylmethyl)-2-methylsulfanyl-1H-pyrimidin-4-one (0.984 mmol, 1 eq) was added in dry vessel. Boron tribromide (2.066 mmol, 2.1 eq) was added and reaction mixture was stirred at 0° C. After 30 min, reaction mixture was allowed to reach to room temperature and it was stirred overnight. Reaction mixture was diluted with water (2 ml). The resulting precipitate, 2-methylsulfanyl-5-(2-oxo-1,2-dihydro-pyrimidin-5-ylmethyl)-1H-pyrimidin-4-one (0.260 mmol, yield=26%) was obtained. 1H NMR (300 MHz, DMSO-d6) δ/ppm 2.45 (s, 3H), 7.75-7.88 (m, 2H), 7.97-8.33 (m, 3H), 11.29-13.09 (m, 4H)

後処理

  1. customEntire reaction
  2. customreaction mixture
  3. customreaction mixture
  4. customto reach to room temperature
  5. stirringit was stirred overnight
  6. customReaction mixture

出典と根拠

ORDレコード
ord-74d371c42a2e48918b09119fa4c3bc8a
出典データセット
uspto-grants-2015_11
特許番号
US09174968B2

反応ノート

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