Solketal → (2,2-Dimethyl-1,3-dioxolan-4-yl)methyl methanesulfonate

HRID 79407ノート

反応式

HRID 79407 の反応式
[CH3:1][C:2]1([CH3:9])[O:6][CH:5]([CH2:7][OH:8])[CH2:4][O:3]1.[CH3:10][S:11](Cl)(=[O:13])=[O:12].C(N(CC)CC)C>C(Cl)Cl>[CH3:10][S:11]([O:8][CH2:7][CH:5]1[CH2:4][O:3][C:2]([CH3:9])([CH3:1])[O:6]1)(=[O:13])=[O:12]

参加物

5

反応物 3

HCID 7528SolketalHCID 8471TriethylamineHCID 31297Methanesulfonyl chloride

生成物 1

HCID 15570840(2,2-Dimethyl-1,3-dioxolan-4-yl)methyl methanesulfonate収率 100.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To (2,2-dimethyl-1,3-dioxolan-4-yl)methanol (400 mg, 3.03 mmol) in DCM (6 mL) at 0° C. was added methanesulfonyl chloride (381 mg, 3.33 mmol) and triethylamine (368 mg, 3.63 mmol. The cold bath was removed and the reaction mixture was stirred for 30 minutes. The mixture was diluted with DCM (5 mL). The organic phase was washed with water (4 mL) and brine (2 mL), and dried (Na2SO4). The solution was concentrated under reduced pressure to give the product (642 mg).

後処理

  1. customThe cold bath was removed
  2. additionThe mixture was diluted with DCM (5 mL)
  3. washThe organic phase was washed with water (4 mL) and brine (2 mL)
  4. dry with materialdried (Na2SO4)
  5. concentrationThe solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-c6973e2a5d534758b3d1c9b5b6305e53
出典データセット
uspto-grants-2014_09
特許番号
US08841455B2

反応ノート

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