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Water → HCID 58306534, 화합물

HRID 1909901
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인쇄 미리보기

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HRID 1909901 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([C:12]([OH:14])=[O:13])[C:10]=1[Cl:11])[N:7](C(OC(C)(C)C)=O)[CH:6]=[CH:5]2.O.C(=O)([O-])[O-].[K+].[K+]>CO>[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([C:12]([OH:14])=[O:13])[C:10]=1[Cl:11])[NH:7][CH:6]=[CH:5]2
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참가 물질

5

반응물 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 58306778HCID 58306778, 화합물

생성물 1

HCID 58306534HCID 58306534, 화합물수율 100.1%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
70 °C

실험 절차

To a mixture of 5-bromo-1-(tert-butoxycarbonyl)-6-chloro-1H-indole-7-carboxylic acid (0.3 g), water (2.0 mL), and methanol (6.0 mL) was added potassium carbonate (0.6 g) at room temperature. The reaction mixture was stirred at 70° C. for 5.5 hours. The reaction mixture was concentrated under reduced pressure, and ethyl acetate and water were added thereto, followed by acidification with 1 M hydrochloric acid. Then, a liquid-separation operation was carried out, and the organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and then evaporated under reduced pressure to obtain 5-bromo-6-chloro-1H-indole-7-carboxylic acid (0.22 g).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and ethyl acetate and water
  2. additionwere added
  3. washthe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-9cc48f31923e46be85c23eb3a8296547
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598355B2

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