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

HRID 45017

반응식

HRID 45017 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-45dd83f459924100b71bdeac030ad732
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541425B2

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