Butylated Hydroxyanisole → HCID 86668285、化合物

HRID 571575

反応式

HRID 571575 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]([CH3:13])([CH3:12])[CH3:11].C(N(CC)CC)C.[CH3:21][S:22](Cl)(=[O:24])=[O:23].C(=O)(O)[O-].[Na+]>C(=O)(OC)OC>[CH3:21][S:22]([O:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]([CH3:13])([CH3:12])[CH3:11])(=[O:24])=[O:23]

参加物

6

反応物 4

HCID 8456Butylated HydroxyanisoleHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 86668285HCID 86668285、化合物収率 76%

試薬・触媒・溶媒 1

HCID 12021Dimethyl Carbonate溶媒

反応条件

温度
25 °C

実験手順

15.0 g (83.2 mmol) of 4-hydroxy-3-tert-butylanisole and 10.5 g (104 mmol) of triethylamine were dissolved in 250 ml of dimethyl carbonate (solvent), and 11.9 g (104 mmol) of methanesulfonyl chloride was dropwise added thereto, taking 25 minutes and controlling the inner temperature at 5° C. or lower. After the addition, this was stirred at 25° C. for 1.5 hours, the reaction mixture was poured into an aqueous saturated sodium bicarbonate solution, the aqueous layer was separated, the organic layer was washed twice with water, and then the organic layer was separated and concentrated. The concentrate was purified through distillation (139° C./32 pa) to give 16.3 g of 2-tert-butyl-4-methoxyphenyl methanesulfonate (yield, 76%).

後処理

  1. customat 5° C.
  2. additionAfter the addition
  3. customthe aqueous layer was separated
  4. washthe organic layer was washed twice with water
  5. customthe organic layer was separated
  6. concentrationconcentrated
  7. distillationThe concentrate was purified through distillation (139° C./32 pa)

出典と根拠

ORDレコード
ord-e6cb5f084f1e46d0a94f4f047535c050
出典データセット
uspto-grants-2015_05
特許番号
US09029024B2

関連ノート

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