Triethylamine → Tert-butyl (4-{2-[(methylsulfonyl)oxy]ethyl}phenoxy)acetate

HRID 898889

反応式

HRID 898889 の反応式
[OH:1][CH2:2][CH2:3][C:4]1[CH:18]=[CH:17][C:7]([O:8][CH2:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])=[CH:6][CH:5]=1.C(N(CC)CC)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28]>C(Cl)Cl>[CH3:26][S:27]([O:1][CH2:2][CH2:3][C:4]1[CH:5]=[CH:6][C:7]([O:8][CH2:9][C:10]([O:12][C:13]([CH3:15])([CH3:14])[CH3:16])=[O:11])=[CH:17][CH:18]=1)(=[O:29])=[O:28]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 23119602Tert-butyl [4-(2-hydroxyethyl)phenoxy]acetate

生成物 1

HCID 86600965Tert-butyl (4-{2-[(methylsulfonyl)oxy]ethyl}phenoxy)acetate収率 95.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-10 °C

実験手順

Tert-butyl [4-(2-hydroxyethyl)phenoxy]acetate (6.000 g, 23.781 mmol) and triethylamine (9.9 ml, 71.341 mmol) were dissolved in DCM. The mixture was cooled to −10° C. and methanesulfonyl chloride (2.8 ml, 35.671 mmol) was added dropwise to the mixture. The reaction mixture was allowed to reach room temperature and was stirred for 16 hours. The mixture was diluted with DCM. The organic layer was washed with water, brine and 0.3M KHSO4, dried with MgSO4, and evaporated under reduced pressure. Obtained 7.5 g of light-yellow crystals (yield 95.5%).

後処理

  1. customto reach room temperature
  2. washThe organic layer was washed with water, brine and 0.3M KHSO4
  3. dry with materialdried with MgSO4
  4. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-645b4593cacc44a79a13e29e22ae538e
出典データセット
uspto-grants-2008_04
特許番号
US07351858B2

関連ノート

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