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Acetic acid, bromo-, diphenylmethyl ester → HCID 13603078、化合物

HRID 2231980
ノート
印刷プレビュー

反応式

HRID 2231980 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.CC(C)([O-])C.[K+].Br[CH2:15][C:16]([O:18][CH:19]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:17]>C1COCC1>[C:20]1([CH:19]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[O:18][C:16]([CH2:15][N:5]2[CH:6]=[CH:7][C:2](=[O:1])[CH:3]=[CH:4]2)=[O:17])[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11130534Acetic acid, bromo-, diphenylmethyl esterHCID 23665647Potassium tert-butoxideHCID 178418642HCID 178418642、化合物

生成物 1

HCID 13603078HCID 13603078、化合物収率 68.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1.37 g of 4-hydroxypyridine was dissolved in 16 ml of THF, then 1.63 g of potassium tert-butoxide was added and reacted overnight. Thereafter, 3.12 g of diphenylmethyl bromoacetate was added and reacted for 6 hours. After the reaction, the solvent was removed, the residue was dissolved in chloroform and washed with water. This was dried over magnesium sulfate, the solvent was removed, and the residue was purified on silica gel chromatography using chloroform-methanol (20:1) to obtain 2.25 g of the title compound (55%).

後処理

  1. customreacted overnight
  2. customreacted for 6 hours
  3. customAfter the reaction
  4. customthe solvent was removed
  5. dissolutionthe residue was dissolved in chloroform
  6. washwashed with water
  7. dry with materialThis was dried over magnesium sulfate
  8. customthe solvent was removed
  9. customthe residue was purified on silica gel chromatography

出典と根拠

ORDレコード
ord-8e8671beed454ee6a77e2b198e0281da
出典データセット
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04785090

反応ノート

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