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Potassium Hydroxide → BN-82451

HRID 2421264
ノート
印刷プレビュー

反応式

HRID 2421264 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 9803928HCID 9803928、化合物

生成物 1

HCID 9905090BN-82451収率 76%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-fa324ad7d8fb41ecbbf165b44d096c76
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07956075B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート