Sodium Hydroxide → HCID 58033225、化合物

HRID 712176ノート

反応式

HRID 712176 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([NH:8][C:9]([NH:11]C(=O)C2C=CC=CC=2)=[S:10])[CH:5]=[C:4]([Br:20])[N:3]=1.[OH-].[Na+].CCOC(C)=O.CCCCCC>C1COCC1.CO.O>[Br:1][C:2]1[CH:7]=[C:6]([NH:8][C:9]([NH2:11])=[S:10])[CH:5]=[C:4]([Br:20])[N:3]=1

参加物

7

反応物 3

HCID 14798Sodium HydroxideHCID 21226206Ethyl acetate hexaneHCID 58033240HCID 58033240、化合物

生成物 1

HCID 58033225HCID 58033225、化合物収率 83%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

To a solution of N-(2,6-dibromopyridin-4-ylcarbamothioyl)benzamide (14.50 g, 34.93 mmol) in a mixture of THF (600 mL) and MeOH (200 mL) was added a solution of NaOH (7.0 g, 174.65 mmol) dissolved in 200 mL of water. The mixture was heated to 70° C. for 16-22 h. After reaction, the solvent wad distilled under reduced pressure, water added and extracted with EtOAc (3×500 mL). The combined organics were washed with brine, dried (Na2SO4), filtered and concentrated under reduced pressure. The residue thus obtained was treated with 20% EtOAc-hexane and finally filtered to obtain the desired product as an off-white solid (9.0 g, 83%).

後処理

  1. customAfter reaction
  2. distillationthe solvent wad distilled under reduced pressure, water
  3. additionadded
  4. extractionextracted with EtOAc (3×500 mL)
  5. washThe combined organics were washed with brine
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue thus obtained
  10. filtrationfinally filtered

出典と根拠

ORDレコード
ord-59823367c329461c96bcdb6a90d1ea43
出典データセット
uspto-grants-2015_11
特許番号
US09181234B2

反応ノート

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