Methanesulfonyl chloride → HCID 22934161, 화합물

HRID 2251894노트

반응식

HRID 2251894 반응식
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:15]=[CH:14][C:10]([CH2:11][CH2:12][OH:13])=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.C(N(C(C)C)CC)(C)C.[CH3:25][S:26](Cl)(=[O:28])=[O:27].C(=O)([O-])O.[Na+]>ClCCl>[S:26]([O:13][CH2:12][CH2:11][C:10]1[CH:9]=[CH:8][C:7]([N:4]2[CH2:3][CH2:2][O:1][CH2:6][CH2:5]2)=[CH:15][CH:14]=1)(=[O:28])(=[O:27])[CH3:25]

참가 물질

6

반응물 4

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 135928032-(4-Morpholinophenyl)ethanol

생성물 1

HCID 22934161HCID 22934161, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

4-Morpholinophenethyl alcohol (2.35 g, 11.3 mmol) was dissolved in dichloromethane (20 ml). Diisopropylethylamine (2.60 ml, 14.8 mmol) and methanesulfonyl chloride (1.11 ml, 14.8 mmol) were added to the obtained solution at 0° C., and they were stirred for 4 hours. The reaction mixture was distributed into 5% aqueous sodium hydrogencarbonate solution and dichloromethane. The organic layer was dried and the solvent was evaporated under reduced pressure. The residue was subjected to the silica gel column chromatography. After the elution with hexane and ethyl acetate (3:1) and then with them (1:1) as the eluents, suitable fractions were collected and the solvent was evaporated under reduced pressure to obtain 4-morpholinophenethyl mesylate in the form of a white solid (2.60 g, 81%).

후처리

  1. customThe organic layer was dried
  2. customthe solvent was evaporated under reduced pressure
  3. washAfter the elution with hexane and ethyl acetate (3:1)
  4. customwith them (1:1) as the eluents, suitable fractions were collected
  5. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-91c790f5238046ea9ba58c09a449558e
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07320973B2

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