Triethylamine → (Tetrahydrofuran-3-yl)methyl methanesulfonate

HRID 1011051ノート

反応式

HRID 1011051 の反応式
[O:1]1[CH2:5][CH2:4][C@@H:3]([CH2:6][OH:7])[CH2:2]1.ClC1N=C2C(N=CN2CC2CCOCC2)=C(Cl)N=1.C(N(CC)CC)C.[CH3:33][S:34](Cl)(=[O:36])=[O:35]>ClCCl>[CH3:33][S:34]([O:7][CH2:6][CH:3]1[CH2:4][CH2:5][O:1][CH2:2]1)(=[O:36])=[O:35]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 40784875((3S)-oxolan-3-yl)methanolHCID 576997032,6-Dichloro-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purine

生成物 1

HCID 22273010(Tetrahydrofuran-3-yl)methyl methanesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To (3S)-tetrahydro-3-furanylmethanol, Isomer 2 (1.4 g) in dry dichloromethane (40 ml) at 0° C. and under nitrogen, was added triethylamine (3.83 ml) followed by methanesulfonyl chloride (1.39 ml). The reaction was stirred at room temperature overnight. The orange solution was diluted with dichloromethane (50 ml) and washed with saturated aqueous sodium bicarbonate (20 ml). The organic layer was separated, dried through a hydrophobic frit and concentrated in vacuo to yield the title compound as an orange oil (2.6 g).

後処理

  1. washwashed with saturated aqueous sodium bicarbonate (20 ml)
  2. customThe organic layer was separated
  3. customdried through a hydrophobic frit
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-0def901c17794d9ea04c6a765e5289bd
出典データセット
uspto-grants-2011_07
特許番号
US07977344B2

反応ノート

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