Potassium Carbonate → Methyl thieno[3,2-c]pyridine-2-carboxylate

HRID 1529481ノート

反応式

HRID 1529481 の反応式
Br[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[CH:8]=O.C([O-])([O-])=O.[K+].[K+].[C:16]([O:20][CH3:21])(=[O:19])[CH2:17][SH:18]>CN(C=O)C.O>[CH3:21][O:20][C:16]([C:17]1[S:18][C:2]2[CH:7]=[CH:6][N:5]=[CH:4][C:3]=2[CH:8]=1)=[O:19]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 16907Methyl ThioglycolateHCID 111167404-Bromopyridine-3-carbaldehyde

生成物 1

HCID 22047666Methyl thieno[3,2-c]pyridine-2-carboxylate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
45 °C

実験手順

To a solution of 4-bromo-pyridine-3-carbaldehyde (1.50 g, 8.06 mmol) in DMF (10 mL) and water (1 mL) was added K2CO3 (1.34 g, 9.68 mmol) and methyl thioglycolate (0.87 mL, 9.68 mmol). The mixture was heated at 45° C. for 18 hours. The reaction mixture was removed from the heating bath and diluted with water (50 mL). After 1 hour, the fluffy solid that formed was filtered and washed with water. The material thus obtained was dried in a 60° C. vacuum oven to a constant weight of 0.92 g (59%). MS m/z 194 (M+H)+.

後処理

  1. customThe reaction mixture was removed from the heating bath
  2. additiondiluted with water (50 mL)
  3. customthe fluffy solid that formed
  4. filtrationwas filtered
  5. washwashed with water
  6. customThe material thus obtained
  7. customwas dried in a 60° C. vacuum oven to a constant weight of 0.92 g (59%)

出典と根拠

ORDレコード
ord-bebb88c4748d48f6a83f58658fc93112
出典データセット
uspto-grants-2015_07
特許番号
US09090625B2

反応ノート

読み込み中…