Sodium Hydroxide → HCID 22282607, 화합물

HRID 2085339노트

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HRID 2085339 반응식
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

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 22282620HCID 22282620, 화합물HCID 23707502Potassium hydroxy sulfite

생성물 1

HCID 22282607HCID 22282607, 화합물수율 91%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8bce0077863d455aad666bf1edec9561
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06720329B2

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