Toluene → Bis(4-butoxyphenyl) sulfide

HRID 1753675

反応式

HRID 1753675 の反応式
Br[CH2:2][CH2:3][CH2:4][CH3:5].[OH:6][C:7]1[CH:12]=[CH:11][C:10]([S:13][C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=2)=[CH:9][CH:8]=1.C(=O)([O-])[O-].[K+].[K+].CN(C=O)C.[C:32]1(C)[CH:37]=CC=[CH:34][CH:33]=1>O>[CH2:2]([O:20][C:17]1[CH:18]=[CH:19][C:14]([S:13][C:10]2[CH:11]=[CH:12][C:7]([O:6][CH2:37][CH2:32][CH2:33][CH3:34])=[CH:8][CH:9]=2)=[CH:15][CH:16]=1)[CH2:3][CH2:4][CH3:5]

参加物

7

反応物 5

HCID 1140TolueneHCID 6228DimethylformamideHCID 8002Butyl bromideHCID 11430Potassium CarbonateHCID 175704,4'-Thiodiphenol

生成物 1

HCID 117666789Bis(4-butoxyphenyl) sulfide収率 99.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution was prepared by combining 107 g of bromobutane, 76 g of bis(4-hydroxyphenyl) sulfide, 108 g of potassium carbonate, and 230 g of DMF. The solution was aged at 90° C. for 16 hours. The aged solution was cooled to room temperature, to which 600 g of water was added to quench the reaction. To the solution was added 300 g of toluene. The organic layer was separated, washed with water, and concentrated in vacuum, obtaining 114 g of the target compound, bis(4-butoxyphenyl) sulfide as amorphous solid. Yield 99%.

後処理

  1. customA solution was prepared
  2. additionwas added
  3. customto quench
  4. customthe reaction
  5. customThe organic layer was separated
  6. washwashed with water
  7. concentrationconcentrated in vacuum

出典と根拠

ORDレコード
ord-607339dd48344dbc9f8a8a7744528260
出典データセット
uspto-grants-2015_10
特許番号
US09164384B2

関連ノート

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