Potassium Hydroxide → HCID 67166457, 화합물

HRID 552378노트

반응식

HRID 552378 반응식
[CH2:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]([NH2:14])[C:5]=1[C:6]([O:8]C)=[O:7])[CH:2]=[CH2:3].[OH-].[K+]>C(O)C>[CH2:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]([NH2:14])[C:5]=1[C:6]([OH:8])=[O:7])[CH:2]=[CH2:3]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 67166341HCID 67166341, 화합물

생성물 1

HCID 67166457HCID 67166457, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of Step 2 intermediate (3.0 g, 15.7 mmol) in ethanol (10 ml) was added 2.0 M potassium hydroxide (4.0 ml) and the mixture was refluxed for 3 h. The mixture was concentrated under reduced pressure and diluted with water. The basic aqueous solution containing the product was washed with diethyl ether (2×25 ml). The aqueous solution was acidified to pH 4.0 with 1N HCl. The solid separated out was filtered and washed with water and dried to give 550 mg of the product as an off-white solid; 1H NMR (δ ppm, CDCl3, 300 MHz): 7.01 (t, J=9.0, 1H); 6.57 (d, J=9.0, 1H); 6.36 (d, J=9.0, 1H); 5.94-5.79 (m, 1H); 5.02-4.90 (m, 2H); 3.46 (d, J=6.0, 2H).

후처리

  1. temperaturethe mixture was refluxed for 3 h
  2. concentrationThe mixture was concentrated under reduced pressure
  3. additiondiluted with water
  4. additionThe basic aqueous solution containing the product
  5. washwas washed with diethyl ether (2×25 ml)
  6. customThe solid separated out
  7. filtrationwas filtered
  8. washwashed with water
  9. customdried

출처 및 근거

ORD 기록
ord-011adf86833f48258e5f6aa0bc4bfe44
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07951814B2

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