Triethylamine → (4-Fluorotetrahydro-2h-pyran-4-yl)methyl methanesulfonate

HRID 624417ノート

反応式

HRID 624417 の反応式
[F:1][C:2]1([CH2:8][OH:9])[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.[CH3:10][S:11](Cl)(=[O:13])=[O:12].C(N(CC)CC)C>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH3:10][S:11]([O:9][CH2:8][C:2]1([F:1])[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1)(=[O:13])=[O:12]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 56971676(4-Fluorooxan-4-yl)methanol

生成物 1

HCID 87279396(4-Fluorotetrahydro-2h-pyran-4-yl)methyl methanesulfonate

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of EXAMPLE 296C (1.4 g), methanesulfonyl chloride (1.054 mL), triethylamine (2.99 mL), and 4-(dimethylamino)pyridine (0.051 g) in CH2Cl2 (20 mL) was stirred at 0° C. for 2 hours, concentrated and chromatographed on silica gel with 30% ethyl acetate in hexanes as eluent to give the product.

後処理

  1. concentrationconcentrated
  2. customchromatographed on silica gel with 30% ethyl acetate in hexanes as eluent
  3. customto give the product

出典と根拠

ORDレコード
ord-71699c738362427ca736016558b29f4c
出典データセット
uspto-grants-2016_04
特許番号
US09303025B2

反応ノート

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