Triethylamine → 1,3-Dimethoxypropan-2-yl methanesulfonate

HRID 1008518ノート

反応式

HRID 1008518 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][O:7][CH2:8][CH:9]([OH:13])[CH2:10][O:11][CH3:12].C(N(CC)CC)C>ClCCl>[CH3:6][O:7][CH2:8][CH:9]([O:13][S:2]([CH3:1])(=[O:4])=[O:3])[CH2:10][O:11][CH3:12]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 121901,3-Dimethoxy-2-propanolHCID 31297Methanesulfonyl chloride

生成物 1

HCID 225957861,3-Dimethoxypropan-2-yl methanesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4.3 mL of methanesulfonyl chloride was added dropwise at 5° C. to a stirred solution of 6.0 g of 1,3-dimethoxy-propan-2-ol and 9.0 mL of triethylamine in 60 mL of dichloromethane. Stirring was continued for 72 hours at room temperature, followed by extraction with water. The combined organic extracts were dried (sodium sulfate) and concentrated and the residue purified by silica chromatography (isohexane/ethyl acetate=9/1, 8/2, 7/3, 6/4 v/v) yielding 2.5 g of methanesulfonic acid 2-methoxy-1-methoxymethyl-ethyl ester as an oil. EI-MS: 198 (M+).

後処理

  1. extractionfollowed by extraction with water
  2. dry with materialThe combined organic extracts were dried (sodium sulfate)
  3. concentrationconcentrated
  4. customthe residue purified by silica chromatography (isohexane/ethyl acetate=9/1, 8/2, 7/3, 6/4 v/v)

出典と根拠

ORDレコード
ord-55a3f9618d2744c69e6d501d32fe95e6
出典データセット
uspto-grants-2004_09
特許番号
US06797710B2

反応ノート

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