Methanesulfonyl chloride → 1,4-Dioxaspiro(4.5)decan-8-yl methanesulfonate

HRID 45017

反応式

HRID 45017 の反応式
[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([OH:11])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.[CH3:12][S:13](Cl)(=[O:15])=[O:14]>C(Cl)(Cl)Cl>[CH3:12][S:13]([O:11][CH:8]1[CH2:9][CH2:10][C:5]2([O:4][CH2:3][CH2:2][O:1]2)[CH2:6][CH2:7]1)(=[O:15])=[O:14]

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 5673521,4-Dioxaspiro(4.5)decan-8-ol

生成物 1

HCID 149667411,4-Dioxaspiro(4.5)decan-8-yl methanesulfonate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
0 °C

実験手順

1,4-Dioxaspiro[4.5]decan-8-ol (0.40 g, 0.0025 mol) was dissolved in chloroform (10.0 mL) and the resulting mixture was cooled at 0° C. To the mixture was added TEA (0.49 mL, 0.0035 mol) and methanesulfonyl chloride (0.23 mL, 0.0030 mol) and this mixture was stirred at 0° C. for 2 hours. The reaction was extracted with ethyl acetate and the organic extracts were washed with water, and saturated NaCl, then dried (MgSO4) and concentrated in vacuo. The crude product was used in the next reaction without further purification.

後処理

  1. extractionThe reaction was extracted with ethyl acetate
  2. washthe organic extracts were washed with water, and saturated NaCl
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. customThe crude product was used in the next reaction without further purification

出典と根拠

ORDレコード
ord-45dd83f459924100b71bdeac030ad732
出典データセット
uspto-grants-2013_09
特許番号
US08541425B2

関連ノート

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