Sodium Hydroxide → 3-{[2-(tetrahydro-2H-pyran-2-yloxy)ethyl]sulfonyl}benzoic acid

HRID 968766ノート

反応式

HRID 968766 の反応式
[S:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([OH:9])=[O:8])([OH:3])=[O:2].[O:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH:14]1[O:19][CH2:20][CH2:21]I.[OH-].[Na+]>O.C(O)C>[O:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH:14]1[O:19][CH2:20][CH2:21][S:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([OH:9])=[O:8])(=[O:3])=[O:2]

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 111186622H-Pyran, tetrahydro-2-(2-iodoethoxy)-HCID 219411183-Sulfinobenzoic acid

生成物 1

HCID 695224113-{[2-(tetrahydro-2H-pyran-2-yloxy)ethyl]sulfonyl}benzoic acid収率 14.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

To a solution of 3-sulfino-benzoic acid (1 g) and 2-iodoethyl tetrahydro-2H-pyran-2-yl ether (1.4 g) in water (20 ml) and ethanol (20 ml) was added NaOH solution to give a pH of 9. The resulting mixture was refluxed for 3 hours before evaporation of the ethanol. The aqueous was acidified to pH3 and the product extracted with EtOAc. The organic layer was separated, dried with MgSO4 and solvent removed by evaporation to give the sub-title compound (0.25 g).

後処理

  1. customto give a pH of 9
  2. extractionthe product extracted with EtOAc
  3. customThe organic layer was separated
  4. dry with materialdried with MgSO4 and solvent
  5. customremoved by evaporation

出典と根拠

ORDレコード
ord-3c23b48ddc334ca4b63f157b93c14c02
出典データセット
uspto-grants-2007_12
特許番号
US07304077B2

反応ノート

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