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Toluene → HCID 59370775, 화합물

HRID 1873975
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인쇄 미리보기

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HRID 1873975 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; Tokyo Chemical Industry, Co., Ltd.) were admixed with each other and stirred overnight at 100° C. The reaction solution was cooled to room temperature, added with toluene and Et2O, and then washed with water three times. The organic layer was dried over magnesium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=84:16→64:36) to obtain the title compound (2.1894 g).

후처리

  1. temperatureThe reaction solution was cooled to room temperature
  2. washwashed with water three times
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. customthe 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-1a01be00f86d4cb0b42a4c69e52e6de8
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08304443B2

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