HCID 19828478、化合物 → HCID 19828471、化合物

HRID 1494526ノート

反応式

HRID 1494526 の反応式
CC1(C)[O:7][CH2:6][C:5]2[C:8]([CH:13]([O:21][C:22](=[O:24])[CH3:23])[C:14]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=3)=[CH:9][N:10]=[C:11]([CH3:12])[C:4]=2[O:3]1>C(O)(C(F)(F)F)=O.O>[CH3:12][C:11]1[C:4]([OH:3])=[C:5]([CH2:6][OH:7])[C:8]([CH:13]([O:21][C:22](=[O:24])[CH3:23])[C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)=[CH:9][N:10]=1

参加物

3

反応物 1

HCID 19828478HCID 19828478、化合物

生成物 1

HCID 19828471HCID 19828471、化合物

試薬・触媒・溶媒 1

HCID 22392675Trifluoroacetic acid water溶媒

実験手順

0.24 g (0.66 mmoles) of (+)-2,2,8-trimethyl-5-(4-chloro-α-acetoxybenzyl)-pyrido-[4,3-e]-1,3-dioxane are poured into a 10 ml round bottomed flask and dissolved in 3.3 ml of TFA/H2O (10:1). The reaction is allowed to stir at room temperature for 1.5 hours, the solvent is then removed by rotary evaporation. 1 ml of methanolic ammonia is added to the crude product (the excess of TFA being neutralized), then evaporated to dryness under high vacuum. The crude product was shown to contain 90% of the desired diol-acetate by HPLC along with 4.4% of unreacted starting material.

後処理

  1. customthe solvent is then removed by rotary evaporation
  2. addition1 ml of methanolic ammonia is added to the crude product (the excess of TFA being
  3. customthen evaporated to dryness under high vacuum

出典と根拠

ORDレコード
ord-8c32e222ef7946a19bc7c28c1fcc9760
出典データセット
uspto-grants-1991_06
特許番号
US05026855

反応ノート

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