Ethyl bromoacetate → HCID 54112137、化合物

HRID 258019ノート

反応式

HRID 258019 の反応式
[OH:1][C:2]1[CH:15]=[C:14]2[C:9]([CH2:10][CH2:11][CH2:12][CH2:13]2)=[C:8]2[C:3]=1[CH2:4][CH2:5][CH2:6][C:7]2=[O:16].Br[CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20].C(=O)([O-])[O-].[K+].[K+]>CC(=O)CC>[CH2:13]1[C:14]2[C:9](=[C:8]3[C:3](=[C:2]([O:1][CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:15]=2)[CH2:4][CH2:5][CH2:6][C:7]3=[O:16])[CH2:10][CH2:11][CH2:12]1

参加物

5

反応物 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 19782189HCID 19782189、化合物

生成物 1

HCID 54112137HCID 54112137、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

40.44 g (0.19 mol) of the compound from Example 6 is heated to reflux with 38.64 g (0.23 mol) of ethyl bromoacetate and 31.97 g (0.23 mol) of potassium carbonate in 190 ml of butanone for 5 h. After cooling, the precipitate is filtered off and washed well with acetone and the solution is evaporated. The residue is taken up in 100 ml of CH2Cl2, shaken 3 times with 50 ml of 10% strength NaOH solution each time, dried over Na2SO4 and evaporated. The residue is dried in a high vacuum.

後処理

  1. temperatureAfter cooling
  2. filtrationthe precipitate is filtered off
  3. washwashed well with acetone
  4. customthe solution is evaporated
  5. dry with materialdried over Na2SO4
  6. customevaporated
  7. customThe residue is dried in a high vacuum

出典と根拠

ORDレコード
ord-a72c69d34e964755b3612b36d928baf5
出典データセット
uspto-grants-1993_11
特許番号
US05264458

反応ノート

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