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Triethylamine → HCID 86666573, 화합물

HRID 2088892
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HRID 2088892 반응식
[OH:1][CH2:2][CH2:3][N:4]1[CH:8]=[C:7]([CH:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)[N:6]=[C:5]1[CH:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH2:16]1.C(N(CC)CC)C.[CH3:35][S:36](Cl)(=[O:38])=[O:37]>ClCCl.C(=O)(O)[O-].[Na+]>[CH3:35][S:36]([O:1][CH2:2][CH2:3][N:4]1[CH:8]=[C:7]([CH:9]2[CH2:10][CH2:11][O:12][CH2:13][CH2:14]2)[N:6]=[C:5]1[CH:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH2:16]1)(=[O:38])=[O:37]
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HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 67113226tert-Butyl 4-(1-(2-hydroxyethyl)-4-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-2-yl)piperidine-1-carboxylate

생성물 1

HCID 86666573HCID 86666573, 화합물수율 95%

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회
HCID 516892
Sodium Bicarbonate
용매

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온도
0 °C

실험 절차

Combine tert-butyl 4-(1-(2-hydroxyethyl)-4-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-2-yl)piperidine-1-carboxylate (4.40 g, 11.60 mmol) and triethylamine (4.9 mL, 3.0 eq) in dichloromethane (72 mL). Cool to 0° C. and add methanesulfonyl chloride (1.1 mL, 1.2 eq). After 1 hour, dilute with additional dichloromethane and saturated aqueous sodium bicarbonate. Separate the layers. Dry the organics over anhydrous sodium sulfate, filter, and concentrate in vacuo to give the title compound as a light yellow solid (5.05 g, 95%). MS (ES) m/z=458 [M]+.

후처리

  1. customSeparate the layers
  2. dry with materialDry the organics over anhydrous sodium sulfate
  3. filtrationfilter
  4. concentrationconcentrate in vacuo

출처 및 근거

ORD 기록
ord-9bc6b42d2e2b4f8691aab4a77e957923
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08436002B2

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