Triethylamine → HCID 18756282, 화합물

HRID 434033

반응식

HRID 434033 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]([F:12])[C:3]=1[C:4](=[N:6][OH:7])Cl.[CH3:13][O:14][C:15](=[O:24])[C:16]#[C:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(N(CC)CC)C>CCOCC.O>[CH3:13][O:14][C:15]([C:16]1[C:4]([C:3]2[C:8]([F:12])=[CH:9][CH:10]=[CH:11][C:2]=2[Cl:1])=[N:6][O:7][C:17]=1[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:24]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 138378Phenylpropynoic acid methyl esterHCID 71367044HCID 71367044, 화합물

생성물 1

HCID 18756282HCID 18756282, 화합물수율 92.2%

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매3회

실험 절차

To a solution of 2-chloro-6-fluorobenzoylchloride oxime (1.04 g, 5.00 mmol) and methyl-3-phenyl-2-propynoate (1.20 g, 7.50 mmol) in Et2O (25 ml) at 0° C. under nitrogen was added a solution of triethyl amine (0.834 ml, 6.00 mmol) in Et2O (3 ml) over 1 h. The reaction was allowed to warm to room temperature overnight (17 h). The mixture was diluted with Et2O and H2O, the layers separated, and the organic fraction was dried (MgSO4). Column chromatography (silica gel, hexane/Et2O gradient) gave the title compound (1.53 g, 92%).

후처리

  1. customthe layers separated
  2. dry with materialthe organic fraction was dried (MgSO4)

출처 및 근거

ORD 기록
ord-438d114149954189898f47939d083395
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06670373B1

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