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Triethylamine → 3-{4-[(Tert-butoxycarbonyl)amino]phenyl}propyl methanesulfonate

HRID 1375724
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HRID 1375724 반응식
[OH:1][CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:18])[O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:7][CH:6]=1.C(N(CC)CC)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28]>C(Cl)Cl>[CH3:26][S:27]([O:1][CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]([O:13][C:14]([CH3:15])([CH3:17])[CH3:16])=[O:18])=[CH:7][CH:6]=1)(=[O:29])=[O:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 219940133-(4-Tert-butoxycarbonylaminophenyl)propanol

생성물 1

HCID 219936273-{4-[(Tert-butoxycarbonyl)amino]phenyl}propyl methanesulfonate수율 92%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

tert-Butyl 4-(3-hydroxypropyl)phenylcarbamate (327 mg, 1.301 mmol) in DCM (15 ml) was cooled in an ice-bath. Triethylamine (0.23 ml, 1.626 mmol) was added, and then methanesulfonyl chloride (164 mg, 1.431 mmol) was added. The mixture was stirred overnight and the temperature was allowed going up to room temperature. It was then washed with water, sodium hydrogencarbonate aqueous solution (1%), water and brine and dried with magnesium sulfate. Evaporation in vacuum to remove the solvent gave the desired product (394 mg), yield 92%.

후처리

  1. customwas allowed going up to room temperature
  2. washIt was then washed with water, sodium hydrogencarbonate aqueous solution (1%), water and brine
  3. dry with materialdried with magnesium sulfate
  4. customEvaporation in vacuum
  5. customto remove the solvent

출처 및 근거

ORD 기록
ord-1e3ee5b0a1664b63aabe94ef44f9b7f0
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07169810B2

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