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Triethylamine → HCID 66968183, 화합물

HRID 549334
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HRID 549334 반응식
[CH2:1]([O:3][C:4](=[O:12])[CH2:5][CH:6]1[CH2:11][O:10][CH2:9][CH2:8][NH:7]1)[CH3:2].C(N(CC)CC)C.[F:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[S:31][C:30]([CH3:32])=[N:29][C:28]=2[C:33](Cl)=[O:34])=[CH:23][CH:22]=1>ClCCl.O>[CH2:1]([O:3][C:4](=[O:12])[CH2:5][CH:6]1[CH2:11][O:10][CH2:9][CH2:8][N:7]1[C:33]([C:28]1[N:29]=[C:30]([CH3:32])[S:31][C:27]=1[C:24]1[CH:25]=[CH:26][C:21]([F:20])=[CH:22][CH:23]=1)=[O:34])[CH3:2]
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 11789040Ethyl 2-(morpholin-3-yl)acetateHCID 223241192-Methyl-5-(4-fluorophenyl)thiazole-4-carbonyl chloride

생성물 1

HCID 66968183HCID 66968183, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

Morpholin-3-ylacetic acid ethyl ester Chem Pharm Bull 94, 31(1), 1983 (2.10 g) was dissolved in dichloromethane (50 ml) and treated with triethylamine (1.33 g). The mixture was cooled (ice bath) and 5-(4-fluoro-phenyl)-2-methyl-thiazole-4-carbonyl chloride (1.53 g) in dichloromethane (10 ml) added. The mixture was stirred for 16 h, diluted with water and the organic phase separated. The aqueous phase was extracted with dichloromethane (2×100 ml), the organic phases combined, dried (Na2SO4) and solvent removed at reduced pressure. the residue was column chromatographed (silica gel, 40% ethyl acetate:pentane ˜60% ethyl acetate pentane eluant) to give the title compound (1.46 g).

후처리

  1. additionadded
  2. customthe organic phase separated
  3. extractionThe aqueous phase was extracted with dichloromethane (2×100 ml)
  4. dry with materialdried (Na2SO4) and solvent
  5. customremoved at reduced pressure
  6. customchromatographed (silica gel, 40% ethyl acetate:pentane ˜60% ethyl acetate pentane eluant)

출처 및 근거

ORD 기록
ord-39468204f0c949e6b1e9896f708fdab9
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07943645B2

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