Triethylamine → 7-(trans-3-Hexadecyloxytetrahydropyran-2-ylmethoxy)heptyl methanesulfonate

HRID 329496ノート

反応式

HRID 329496 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH2:6]([O:22][C@@H:23]1[CH2:28][CH2:27][CH2:26][O:25][C@H:24]1[CH2:29][O:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][OH:38])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21].C(N(CC)CC)C>C1C=CC=CC=1>[CH3:1][S:2]([O:38][CH2:37][CH2:36][CH2:35][CH2:34][CH2:33][CH2:32][CH2:31][O:30][CH2:29][C@H:24]1[C@H:23]([O:22][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:28][CH2:27][CH2:26][O:25]1)(=[O:4])=[O:3]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 186371307-(trans-3-Hexadecyloxytetrahydropyran-2-yl)methoxy-1-heptanol

生成物 1

HCID 186371317-(trans-3-Hexadecyloxytetrahydropyran-2-ylmethoxy)heptyl methanesulfonate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

A solution of 0.51 ml of methanesulfonyl chloride dissolved in 5 ml of benzene was added dropwise to a solution of 2.067 g of dl-7-(trans-3-hexadecyloxytetrahydropyran-2-ylmethoxy)-1-heptanol (prepared as described in Preparation 55) and 1.83 ml of triethylamine dissolved in 15 ml of benzene, whilst ice-cooling. The reaction mixture was stirred at room temperature for 15 minutes, after which it was washed with water, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure, to give 2.406 g of crude dl-7-(trans-3-hexadecyloxytetrahydropyran-2-ylmethoxy)heptyl methanesulfonate as a viscous oil.

後処理

  1. temperaturecooling
  2. washafter which it was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-56be040bd29747c49bb4e92ab4e45241
出典データセット
uspto-grants-1990_01
特許番号
US04891363

反応ノート

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