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Sulfuric Acid → HCID 23149682、化合物

HRID 555676
ノート
印刷プレビュー

反応式

HRID 555676 の反応式
[C:1]12([C:12]([O:14][CH3:15])=[O:13])[CH2:8][CH2:7][C:4]([C:9]([OH:11])=[O:10])([CH2:5][CH2:6]1)[CH2:3][CH2:2]2.S(=O)(=O)(O)O>ClCCl>[C:4]12([C:9]([O:11][C:1]([CH3:8])([CH3:6])[CH3:2])=[O:10])[CH2:3][CH2:2][C:1]([C:12]([O:14][CH3:15])=[O:13])([CH2:6][CH2:5]1)[CH2:8][CH2:7]2
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 1118Sulfuric AcidHCID 110420624-(Methoxycarbonyl)bicyclo[2.2.2]octane-1-carboxylic acid

生成物 1

HCID 23149682HCID 23149682、化合物収率 157.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Methyl hydrogen bicyclo[2.2.2]octane-1,4-dicarboxylate (500 mg) was dissolved in dichloromethane (5 mL) and sulfuric acid (50 μL) was added to the solution. The mixture was bubbled with isobutene for 5 minutes while chilled in a salt/ice bath. The mixture was then stirred for 4 hours at room temperature and was left for 4 days. Subsequently, the reaction mixture was diluted with dichloromethane (5 mL), washed sequentially with a saturated aqueous solution of sodium bicarbonate and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was dried under reduced pressure to give 1,1-dimethylethyl methyl bicyclo[2.2.2]octane-1,4-dicarboxylate (497 mg).

後処理

  1. customThe mixture was bubbled with isobutene for 5 minutes
  2. temperaturewhile chilled in a salt/ice bath
  3. waitwas left for 4 days
  4. additionSubsequently, the reaction mixture was diluted with dichloromethane (5 mL)
  5. washwashed sequentially with a saturated aqueous solution of sodium bicarbonate and saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was dried under reduced pressure

出典と根拠

ORDレコード
ord-8b5f4acfc1e84fd582f0b6042e60787a
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08053465B2

反応ノート

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