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Triethylamine → 2-(Tetrahydro-3-furanyl)ethyl methanesulfonate

HRID 1010990
ノート
印刷プレビュー

反応式

HRID 1010990 の反応式
[O:1]1[CH2:5][CH2:4][CH:3]([CH2:6][CH2:7][OH:8])[CH2:2]1.C(N(CC)CC)C.[CH3:16][S:17](Cl)(=[O:19])=[O:18].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[CH3:16][S:17]([O:8][CH2:7][CH2:6][CH:3]1[CH2:4][CH2:5][O:1][CH2:2]1)(=[O:19])=[O:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 111262252-(Oxolan-3-yl)ethan-1-ol

生成物 1

HCID 576998222-(Tetrahydro-3-furanyl)ethyl methanesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

このページの内容参加物実験手順後処理出典と根拠反応ノート

2-(Tetrahydro-3-furanyl)ethanol (230 mg) was dissolved in dry DCM (5 mL) and triethylamine (0.552 mL) was added. The stirred solution was cooled (ice bath) under nitrogen and methanesulphonyl chloride (0.199 mL) was added dropwise over 5 mins. The mixture was allowed to warm slowly to room temperature as the ice bath melted and was left for 16 h. The mixture was shaken with saturated sodium bicarbonate solution and the aqueous layer was extracted with DCM (×2). The combined organics were washed with brine, dried using a hydrophobic frit and evaporated to give the title compound (364 mg).

後処理

  1. temperatureThe stirred solution was cooled (ice bath) under nitrogen
  2. extractionthe aqueous layer was extracted with DCM (×2)
  3. washThe combined organics were washed with brine
  4. customdried
  5. customevaporated

出典と根拠

ORDレコード
ord-6d6052d02976479ead74394d279bfd66
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977344B2

反応ノート

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