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Potassium Hydroxide → BN-82451

HRID 2065963
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HRID 2065963 반응식
[OH-].[K+].[C:3]([C:7]1[CH:8]=[C:9]([C:18]2[N:19]=[C:20]([CH2:23][NH:24]C(=O)OCC3C=CC=CC=3)[S:21][CH:22]=2)[CH:10]=[C:11]([C:14]([CH3:17])([CH3:16])[CH3:15])[C:12]=1[OH:13])([CH3:6])([CH3:5])[CH3:4]>CO>[NH2:24][CH2:23][C:20]1[S:21][CH:22]=[C:18]([C:9]2[CH:10]=[C:11]([C:14]([CH3:15])([CH3:16])[CH3:17])[C:12]([OH:13])=[C:7]([C:3]([CH3:6])([CH3:5])[CH3:4])[CH:8]=2)[N:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 9803928HCID 9803928, 화합물

생성물 1

HCID 9905090BN-82451수율 76%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

0.1 ml of a 40% solution of potassium hydroxide is added dropwise to a solution of 0.106 g (1.1 mmol) of the compound of Example 10 in 10 ml of methanol. After overnight stirring under reflux, the reaction mixture is concentrated under vacuum and the residue is diluted with dichloromethane and washed with a 1N solution of HCl then with 50 ml of a saturated solution of NaCl. The organic phase is separated and dried over magnesium sulphate, filtered and concentrated under vacuum. The expected product is obtained after chromatography on a silica column (eluent: 5% ethanol in dichloromethane) in the form of a brown foam with a yield of 76%.

후처리

  1. temperatureunder reflux
  2. concentrationthe reaction mixture is concentrated under vacuum
  3. additionthe residue is diluted with dichloromethane
  4. washwashed with a 1N solution of HCl
  5. customThe organic phase is separated
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-9028da00da8e464fa2c2750e6e21ba14
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288560B2

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