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4-Toluenesulfonyl chloride → HCID 87269179, 화합물

HRID 1516058
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HRID 1516058 반응식
C([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8]([O:13][CH2:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH:23]([OH:25])[CH3:24])=[CH:17][CH:16]=2)[CH:7]=[N:6]1)(C)(C)C.[S:26](Cl)([C:29]1[CH:35]=[CH:34][C:32]([CH3:33])=[CH:31][CH:30]=1)(=[O:28])=[O:27].[CH2:37](N(CC)CC)C.CC[CH2:46][CH2:47][CH3:48]>ClCCl.CN(C1C=CN=CC=1)C.O.C(OCC)(=O)C>[C:47]([CH:14]([O:13][C:8]1[CH:7]=[N:6][NH:5][C:10](=[O:11])[C:9]=1[Cl:12])[C:15]1[CH:16]=[CH:17][C:18]([O:21][CH2:22][CH:23]([O:25][S:26]([C:29]2[CH:35]=[CH:34][C:32]([CH3:33])=[CH:31][CH:30]=2)(=[O:28])=[O:27])[CH3:24])=[CH:19][CH:20]=1)([CH3:46])([CH3:48])[CH3:37]
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참가 물질

9

반응물 4

HCID 73974-Toluenesulfonyl chlorideHCID 8003PentaneHCID 8471TriethylamineHCID 59678685HCID 59678685, 화합물

생성물 1

HCID 87269179HCID 87269179, 화합물수율 58%

시약·촉매·용매 4

HCID 142844-(Dimethylamino)pyridine촉매
HCID 962
Water
용매
HCID 6344Dichloromethane용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of the product of Example 6C (200 mg, 0.546 mmol) dissolved in anhydrous dichloromethane (6.0 mL) was added TsCl (125 mg, 0.656 mmol), DMAP (100 mg, 0.819 mmol) and triethylamine (0.0914 mL, 0.656 mmol). The reaction mixture continued stirring at room temperature. After 22 hours the reaction mixture was diluted with water. The aqueous layer was separated and extracted with ethyl acetate (3×). All combined organic layers were dried over Na2SO4, filtered, and concentrated to provide an oil. The crude material was purified using silica gel:chromatography (70:30 pentane:ethyl acetate) to provide the desired product (166 mg, 0.319 mmol) in 58% yield. 1H (CDCl37.80 (2H, d, 600 MHz): δ J=8.3 Hz), 7.72 (1H, s), 7.32 (2H, d, J=7.9 Hz), 7.29 (2H, d, J=8.7 Hz), 6.74 (2H, d, J=8.7 Hz), 5.22 (2H, s), 4.19 (1H, m), 4.02 (1H, dd, J=10.4, 6.0 Hz), 3.93 (1H, dd, J=10.4, 4.5 Hz), 2.44 (3H, s), 1.63 (9H, s) 1.42 (3H, d, J=6.5 Hz); 13C (CDCl3 158.9, 150 MHz): δ 158.3, 153.6, 144.6, 133.8, 129.6, 128.8, 127.8, 127.4, 125.1, 118.0, 114.7, 76.8, 71.5, 69.7, 66.2, 27.7, 21.5, 17.6.; HRMS calcd for C25H29ClN2O6S: 521.150762, found 521.1505.

후처리

  1. customThe aqueous layer was separated
  2. extractionextracted with ethyl acetate (3×)
  3. dry with materialAll combined organic layers were dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto provide an oil
  7. customThe crude material was purified

출처 및 근거

ORD 기록
ord-d0fcdb825a8f430da23b134cd088858e
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08226929B2

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