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HCID 22341850、化合物 → HCID 22182264、化合物

HRID 749320
ノート
印刷プレビュー

反応式

HRID 749320 の反応式
[CH3:1][C:2]1([CH3:13])[CH2:7][C:6](=[O:8])[CH2:5][C:4]([CH2:11][CH3:12])([CH2:9][CH3:10])[NH:3]1>CO>[CH3:13][C:2]1([CH3:1])[CH2:7][CH:6]([OH:8])[CH2:5][C:4]([CH2:9][CH3:10])([CH2:11][CH3:12])[NH:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 22341850HCID 22341850、化合物

生成物 1

HCID 22182264HCID 22182264、化合物収率 99.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of 15.8 g (0.086 mol) 2,2-dimethyl-6,6diethyl-4-oxopiperidine In 50 ml methanol 2.2 g (0.06 M) sodium borohydride are acided in portions. The temperature is kept below 30° C. After stirring over night methanol is removed under vacuum and the residue is diluted with 20 ml 2N-NaOH. The solution is extracted with ethylacetate. The combined extracts are washed with saturated NaCl solution, dried over MgSO4 and dried under vacuum at 60° C./50 mbar until a constant weight is achieved. 15.8 g (99%) 2,2-dimethyl-6,6-diethyl-4-hydroxypiperidine are obtained as yellowish oil. :

後処理

  1. customis kept below 30° C
  2. customis removed under vacuum
  3. additionthe residue is diluted with 20 ml 2N-NaOH
  4. extractionThe solution is extracted with ethylacetate
  5. washThe combined extracts are washed with saturated NaCl solution
  6. dry with materialdried over MgSO4
  7. customdried under vacuum at 60° C./50 mbar until a constant weight

出典と根拠

ORDレコード
ord-576b029e3eae4e03b2fef7825718fcb1
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07402639B2

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