Water → HCID 565576、化合物

HRID 1956126ノート

反応式

HRID 1956126 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1([CH3:19])[C:12]2([C:16](O)=[O:17])[C:13]([CH2:15][CH:9]1[CH2:10][CH2:11]2)=[O:14].O>CCOCC>[CH3:7][C:8]1([CH3:19])[CH:9]2[CH2:10][CH2:11][C:12]1([CH2:16][OH:17])[CH:13]([OH:14])[CH2:15]2

参加物

5

反応物 3

HCID 962WaterHCID 2978887,7-Dimethyl-2-oxobicyclo[2.2.1]heptane-1-carboxylic acidHCID 21226445Aluminium lithium hydride

生成物 1

HCID 565576HCID 565576、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To an ice-cooled mixture of lithium aluminum hydride (4 g, 105.4 mmol) in ether was added dropwise a solution of camphorsulfonyl chloride (10 g, 39.88 mmol) and ketopinic acid, prepared as described in Step 1, above. After the addition was complete, the ice bath was removed and the mixture was stirred at ambient temperature for 2 hrs. The mixture was cooled again and wet ether was added cautiously. When the violent reaction subsided, water was added. The mixture was then extracted three times with ethyl acetate. The combined extracts were washed with water and brine and dried over anhydrous magnesium sulfate. Evaporation of the solution gave 4.8 g of a white powder. NMR(δ): 0.90 (s, 3H), 1.20 (s, 3H).

後処理

  1. customprepared
  2. additionAfter the addition
  3. customthe ice bath was removed
  4. temperatureThe mixture was cooled again
  5. additionwet ether was added cautiously
  6. customWhen the violent reaction
  7. extractionThe mixture was then extracted three times with ethyl acetate
  8. washThe combined extracts were washed with water and brine
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customEvaporation of the solution

出典と根拠

ORDレコード
ord-8c51aa3af364458487c466c1c1afd148
出典データセット
uspto-grants-1998_07
特許番号
US05780249

反応ノート

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