Sodium Hydroxide → 4-But-2-ynyloxy-benzenesulfonic acid sodium salt

HRID 1264611ノート

反応式

HRID 1264611 の反応式
[Na+:1].[OH:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([O-:12])(=[O:11])=[O:10])=[CH:5][CH:4]=1.[OH-].[Na+].Br[CH2:16][C:17]#[C:18][CH3:19]>C(O)(C)C>[Na+:1].[CH2:16]([O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([O-:12])(=[O:10])=[O:11])=[CH:5][CH:4]=1)[C:17]#[C:18][CH3:19]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 27568621-Bromo-2-butyneHCID 4379756Sodium 4-hydroxybenzenesulfonate

生成物 1

HCID 237040564-But-2-ynyloxy-benzenesulfonic acid sodium salt収率 100.3%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

To a solution of 52.35 g (0.225 mol) of 4-hydroxybenzenesulfonate sodium salt in 1L of isopropanol and 225 mL of a 1.0N solution of sodium hydroxide was added 59.96 g (0.45 mol) of 1-bromo-2-butyne. The resulting mixture was heated to 70° for 15 h and then the isopropanol was removed by evaporation in vacuo. The resulting white precipitate was collected by filtration, washed with isopropanol and ether and dried under vacuum to give 56.0 g (100%) of 4-but-2-ynyloxybenzenesulfonic acid sodium salt as a white solid.

後処理

  1. temperatureThe resulting mixture was heated to 70° for 15 h
  2. customthe isopropanol was removed by evaporation in vacuo
  3. filtrationThe resulting white precipitate was collected by filtration
  4. washwashed with isopropanol and ether
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-a8d93a5748d14508a25d7cfa4e1d58b9
出典データセット
uspto-grants-2003_04
特許番号
US06544984B1

反応ノート

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