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Diisopropylethylamine → HCID 178437207, 화합물

HRID 706042
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HRID 706042 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15]Cl)=[CH:11][CH:10]=2)=[CH:4][C:3]=1[C:17]([F:20])([F:19])[F:18].[CH2:21]([C:23]1[C:24](=[O:30])[NH:25][C:26](=[S:29])[NH:27][CH:28]=1)[CH3:22].CCN(C(C)C)C(C)C>ClCCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][S:29][C:26]3[NH:27][CH:28]=[C:23]([CH2:21][CH3:22])[C:24](=[O:30])[N:25]=3)=[CH:11][CH:10]=2)=[CH:4][C:3]=1[C:17]([F:20])([F:19])[F:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 30020425-Ethyl-2-thiouracilHCID 668255374-(Chloromethyl)phenyl 4-chloro-3-(trifluoromethyl)phenyl ether

생성물 1

HCID 178437207HCID 178437207, 화합물수율 46%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

A mixture of 1-chloro-4-{[4-(chloromethyl)phenyl]oxy}-2-(trifluoromethyl)benzene (65 mg, 0.202 mmol), 5-ethyl-2-thioxo-2,3-dihydro-4(1H)-pyrimidinone (47.4 mg, 0.304 mmol) and DIPEA (0.163 mL, 0.933 mmol) in DCE (3.0 mL) was sealed in a vessel and stirred at room temperature for 5 min, then was heated with a microwave condition at 80° C. for 30 min. After cooling, the reaction was quenched with water, extracted with EA, the combined organic layers were dried with sodium sulfate, concentrated, and purified via MDAP to afford the title compound (41 mg, 45.9% yield). LCMS: rt=3.94 min, [M+H+]=441

후처리

  1. customwas sealed in a vessel
  2. temperaturewas heated with a microwave condition at 80° C. for 30 min
  3. temperatureAfter cooling
  4. customthe reaction was quenched with water
  5. extractionextracted with EA
  6. dry with materialthe combined organic layers were dried with sodium sulfate
  7. concentrationconcentrated
  8. custompurified via MDAP

출처 및 근거

ORD 기록
ord-3d9eb5c7b0484a23b3e16c5aa461fff3
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09174968B2

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