Sodium Carbonate → Mellein

HRID 594923ノート

反応式

HRID 594923 の反応式
CCCCCCCCCCCCCCCCCCN[C:20]([CH2:22][CH2:23][C:24]1[CH:29]=[C:28](C(C)(C)C)[C:27](O)=[C:26](C(C)(C)C)[CH:25]=1)=O.[O-:39][Mn](=O)(=O)=O.[K+].[C:45]([O-])([O-:47])=[O:46].[Na+].[Na+]>CC(O)=O.O>[CH3:20][CH:22]1[O:47][C:45](=[O:46])[C:29]2[C:28]([OH:39])=[CH:27][CH:26]=[CH:25][C:24]=2[CH2:23]1

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 516875Potassium PermanganateHCID 197363073,5-Bis(1,1-dimethylethyl)-4-hydroxy-N-octadecylbenzenepropanamide

生成物 1

HCID 28516Mellein

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

実験手順

To a stirred solution of AO-1 (16.5 g, 83.0 mmol) in AcOH (150 mL) kept below 10° C. is added a solution of KMnO4 (14.5 g, 92.0 mmol) in H2O (150 mL) dropwise. The reaction mixture is stirred for 30 min. The mixture is diluted with water, basified by addition of saturated aq Na2CO3 and extracted with EtOAc. The solution is concentrated and the residue is purified by SFC to yield AO-2.

後処理

  1. customkept below 10° C.
  2. extractionextracted with EtOAc
  3. concentrationThe solution is concentrated
  4. customthe residue is purified by SFC

出典と根拠

ORDレコード
ord-d400661187fc4bccad7895e0d676b0bc
出典データセット
uspto-grants-2016_01
特許番号
US09242989B2

反応ノート

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