Potassium Hydroxide → HCID 67166457、化合物

HRID 552378ノート

反応式

HRID 552378 の反応式
[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]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 67166341HCID 67166341、化合物

生成物 1

HCID 67166457HCID 67166457、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-011adf86833f48258e5f6aa0bc4bfe44
出典データセット
uspto-grants-2011_05
特許番号
US07951814B2

反応ノート

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