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Toluene → HCID 59370775, 화합물

HRID 1678722
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인쇄 미리보기

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HRID 1678722 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([O:11][Si:12]([CH2:17][CH3:18])([CH2:15][CH3:16])[CH2:13][CH3:14])[CH2:9]I)=[CH:4][C:3]=1[NH:19][S:20]([CH3:23])(=[O:22])=[O:21].[CH2:24]([NH:31][CH2:32][CH2:33][OH:34])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C1(C)C=CC=CC=1>CCOCC>[CH2:24]([N:31]([CH2:32][CH2:33][OH:34])[CH2:9][C@@H:8]([C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([NH:19][S:20]([CH3:23])(=[O:22])=[O:21])[CH:4]=1)[O:11][Si:12]([CH2:17][CH3:18])([CH2:15][CH3:16])[CH2:13][CH3:14])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1
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참가 물질

5

반응물 3

HCID 1140TolueneHCID 4348BenzylethanolamineHCID 53922285HCID 53922285, 화합물

생성물 1

HCID 59370775HCID 59370775, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
100 °C

실험 절차

(R)-N-(2-chloro-5-(2-iodo-1-(triethylsilyloxy)ethyl)phenyl)methanesulfonamide (3 g) and 2-(benzylamino)ethanol (6 mL; manufactured by Tokyo Chemical Industry Co., Ltd.) were mixed, and the mixture was stirred overnight at 100° C. The reaction solution was cooled to room temperature, and then toluene and Et2O were added thereto. The mixture was washed three times with water, and the organic layer was dried over magnesium sulfate. Then, the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=84:16→64:36), and thus the title compound (2.1894 g) was obtained.

후처리

  1. temperatureThe reaction solution was cooled to room temperature
  2. washThe mixture was washed three times with water
  3. dry with materialthe organic layer was dried over magnesium sulfate
  4. customThen, the solvent was evaporated under reduced pressure
  5. customThe residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=84:16→64:36)

출처 및 근거

ORD 기록
ord-202e718141cf426db488aea094d95910
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08008506B2

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