Tetrabutylammonium Fluoride → 1-(2-Hydroxyethyl)-2,5-dimethoxy-3,6-bis(methoxymethoxy)benzene

HRID 1588135ノート

反応式

HRID 1588135 の反応式
[Si]([O:8][CH2:9][CH2:10][C:11]1[C:16]([O:17][CH2:18][O:19][CH3:20])=[C:15]([O:21][CH3:22])[CH:14]=[C:13]([O:23][CH2:24][O:25][CH3:26])[C:12]=1[O:27][CH3:28])(C(C)(C)C)(C)C.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1>[OH:8][CH2:9][CH2:10][C:11]1[C:16]([O:17][CH2:18][O:19][CH3:20])=[C:15]([O:21][CH3:22])[CH:14]=[C:13]([O:23][CH2:24][O:25][CH3:26])[C:12]=1[O:27][CH3:28]

参加物

4

反応物 2

HCID 2724141Tetrabutylammonium FluorideHCID 197572472-[2,5-Dimethoxy-3,6-bis(methoxymethoxy)phenyl]ethyl tert-butyldimethylsilyl ether

生成物 1

HCID 137145691-(2-Hydroxyethyl)-2,5-dimethoxy-3,6-bis(methoxymethoxy)benzene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

15.0 Milligrams of 2-[2,5-dimethoxy-3,6-bis(methoxymethoxy)phenyl]ethyl tert-butyldimethylsilyl ether was dissolved in 2 ml of anhydrous tetrahydrofuran, under argon gas stream conditions, 0.1 ml of tetrahydrofuran solution of 1 mole of tetra-n-butylammonium fluoride was added thereto and stirred for 30 minutes, the reaction of removal of the protecting group was completed quantitatively. The solvent was removed by evaporation under reduced pressure, and the residue obtained was treated on a silica gel thin layer chromatography and purified by developing with 30% ethyl acetate-n-hexane to yield 9.0 mg of 1-(2-hydroxyethyl)-2,5-dimethoxy-3,6-bis(methoxymethoxy)benzene.

後処理

  1. additionwas added
  2. customthe reaction of removal of the protecting group
  3. customThe solvent was removed by evaporation under reduced pressure
  4. customthe residue obtained
  5. additionwas treated on a silica gel thin layer chromatography
  6. custompurified

出典と根拠

ORDレコード
ord-cfbe83558bc4444ba32710253b9d5b76
出典データセット
uspto-grants-1993_06
特許番号
US05220042

反応ノート

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