Sodium Hydroxide → HCID 11728935、化合物

HRID 1637206ノート

反応式

HRID 1637206 の反応式
[OH-].[Na+].[C:3]1([S:9][C:10]2[C:11]3[CH:23]=[CH:22][C:21]([O:24][CH2:25][C:26]4[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=4)=[CH:20][C:12]=3[S:13][C:14]=2[C:15]([O:17]CC)=[O:16])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>O1CCOCC1>[C:3]1([S:9][C:10]2[C:11]3[CH:23]=[CH:22][C:21]([O:24][CH2:25][C:26]4[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=4)=[CH:20][C:12]=3[S:13][C:14]=2[C:15]([OH:17])=[O:16])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 9931973HCID 9931973、化合物

生成物 1

HCID 11728935HCID 11728935、化合物収率 79.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

Sodium hydroxide (0.5 ml of 2M in water) was added to a solution of ethyl 3-(phenylsulfanyl)-6-(3-pyridylmethoxy)benzo[b]thiophene-2-carboxylate (Example 1, 190 mg, 0.45 mmol) in 1,4-dioxane, and the mixture heated to 60° C. for 4 hours. The solvents were removed under reduced pressure, and the residue was dissolved in water (15 ml) and washed with ethyl acetate (25 ml). The aqueous layer was separated and acidified by dropwise addition of acetic acid until a white solid precipitated. The solid was isolated by filtration and dried under vacuo to give the title compound as a colourless solid (140 mg).

後処理

  1. customThe solvents were removed under reduced pressure
  2. dissolutionthe residue was dissolved in water (15 ml)
  3. washwashed with ethyl acetate (25 ml)
  4. customThe aqueous layer was separated
  5. additionacidified by dropwise addition of acetic acid until a white solid
  6. customprecipitated
  7. customThe solid was isolated by filtration
  8. customdried under vacuo

出典と根拠

ORDレコード
ord-3e8b41e8ee1d4fa68f1ba0a8a7e1524d
出典データセット
uspto-grants-2000_03
特許番号
US06040309

反応ノート

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