Sodium Hydroxide → HCID 22282607、化合物

HRID 2085339ノート

反応式

HRID 2085339 の反応式
S1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[C:4]([C:11]2[CH:20]=[CH:19][C:14]([C:15]([O:17][CH3:18])=[O:16])=[CH:13][CH:12]=2)=[CH:3][CH2:2]1.O[O:22][S:23]([O-:25])=O.[K+].[OH-].[Na+]>CO.O>[O:22]=[S:23]1(=[O:25])[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[C:4]([C:11]2[CH:12]=[CH:13][C:14]([C:15]([O:17][CH3:18])=[O:16])=[CH:19][CH:20]=2)=[CH:3][CH2:2]1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 22282620HCID 22282620、化合物HCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 22282607HCID 22282607、化合物収率 91%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

反応条件

温度
0 °C

実験手順

Methyl 4-(2H-1-benzothiopyran-4-yl)benzoate from reaction 33b (0.77 g, 2.75 mmol) was dissolved in methanol (30 mL) cooled to 0° C. and Oxone® (6.76 g, 11.1 mmol) in water (7 mL) was added. The reaction was stirred for 1 h at 0° C. and then allowed to warm to room temperature and stir for another hour. The reaction was diluted with water, pH adjusted to pH=8 with 1 N sodium hydroxide. This was extracted with ethyl acetate. The combined organic layers were washed with water, brine, dried over magnesium sulfate and concentrated to give methyl 4-(1,1-dioxido-2H-1-benzothiopyran-4-yl)benzoate (0.784 g, 91%) as a solid.

後処理

  1. temperatureto warm to room temperature
  2. stirringstir for another hour
  3. extractionThis was extracted with ethyl acetate
  4. washThe combined organic layers were washed with water, brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-8bce0077863d455aad666bf1edec9561
出典データセット
uspto-grants-2004_04
特許番号
US06720329B2

反応ノート

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