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Triethylamine → (+/-)-1-Methoxy-2-butanol Methanesulfonate

HRID 1279269
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HRID 1279269 반응식
[CH3:1][O:2][CH2:3][CH:4]([OH:7])[CH2:5][CH3:6].CCN(CC)CC.[CH3:15][S:16](Cl)(=[O:18])=[O:17]>C(Cl)Cl>[CH3:15][S:16]([O:7][CH:4]([CH2:5][CH3:6])[CH2:3][O:2][CH3:1])(=[O:18])=[O:17]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 408952-Butanol, 1-methoxy-

생성물 1

HCID 22273165(+/-)-1-Methoxy-2-butanol Methanesulfonate수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
25 °C

실험 절차

A solution of 1-methoxy-2-butanol (52.08 g, 57.23 mL, 0.5 mol) and Et3N (108.2 mL, 0.75 mol, 1.5 equiv) in CH2Cl2 (500 mL) was treated dropwise with methanesulfonyl chloride (68.73 g, 46.44 mL, 0.6 mol, 1.2 equiv) at 0° C. under N2. The reaction mixture was warmed to 25° C. and stirred at 25° C. for an additional 4 h before being quenched with H2O (300 mL). The two layers were separated, and the aqueuos was extracted with CH2Cl2 (3×100 mL). The combined CH2Cl2 extracts were washed with H2O (2×200 mL) and saturated aqueuos NaCl (200 mL), dried (MgSO4), and concentrated in vacuo. The residue was dried enough in vacuo to afforded the desired mesylate 1 (85-90.0 g, 91 g theoretical, 93-98%) as a pale-yellow oil, which was pure enough and directly used in the next reaction without further purification.

후처리

  1. custombefore being quenched with H2O (300 mL)
  2. customThe two layers were separated
  3. extractionthe aqueuos was extracted with CH2Cl2 (3×100 mL)
  4. washThe combined CH2Cl2 extracts were washed with H2O (2×200 mL) and saturated aqueuos NaCl (200 mL)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customThe residue was dried enough in vacuo

출처 및 근거

ORD 기록
ord-fb8dbab707ca4bdeb61c800292570c50
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06448261B1

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