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Water → HCID 59201345, 화합물

HRID 451687
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HRID 451687 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9]([O:23][CH2:24][CH2:25][OH:26])[C@@H:10]1[CH2:15][CH2:14][CH2:13][N:12]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:11]1.CCN(CC)CC.[CH3:34][S:35](Cl)(=[O:37])=[O:36].O>C(Cl)Cl>[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9]([O:23][CH2:24][CH2:25][O:26][S:35]([CH3:34])(=[O:37])=[O:36])[C@@H:10]1[CH2:15][CH2:14][CH2:13][N:12]([C:16]([O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:17])[CH2:11]1
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참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 59201577HCID 59201577, 화합물

생성물 1

HCID 59201345HCID 59201345, 화합물수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of (3R)-tert-butyl 3-((2,3-difluorophenyl)(2-hydroxyethoxy)methyl)piperidine-1-carboxylate in dry CH2Cl2 (50 mL) was added Et3N (5.2 mL, 37.6 mmol) at −5-0° C. Then a solution of MsCl (1.3 g, 11.3 mmol) in dry CH2Cl2 (20 mL) was added dropwise at the same temperature. After addition, the reaction was allowed to gradually warm to rt. Upon completion of the reaction, 50 mL of water was added, the aqueous layer was extracted with CH2Cl2, the combined organic layers were washed with 10% citric acid, sat. NaHCO3 and brine, then dried over Na2SO4, filtered and concentrated to give (3R)-tert-butyl 3-((2,3-difluorophenyl)(2-(methylsulfonyloxy)ethoxy)methyl)piperidine-1-carboxylate (4.2 g, 99%), which was used in the next step without purification. 1H NMR (CDCl3, 400 MHz) δ 7.12 (m, 3H), 4.52 (q, 1H), 4.31 (m, 3H), 4.09 (t, 1H), 3.57 (m, 2H), 3.06 (d, 3H), 2.70 (m, 2H), 1.93 (m, 2H), 1.44 (d, 9H).

후처리

  1. additionAfter addition
  2. additionwas added
  3. extractionthe aqueous layer was extracted with CH2Cl2
  4. washthe combined organic layers were washed with 10% citric acid, sat. NaHCO3 and brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0e14c32fd9cf435aa43ce99bc315faba
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08487108B2

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