Triethylamine → HCID 59750346, 화합물

HRID 748161노트

반응식

HRID 748161 반응식
[C:1]([O:10]C)(=O)[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[SH:4].[CH:12]([O:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]#[N:23])=[CH:18][N:17]=1)([CH3:14])[CH3:13].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH:12]([O:15][C:16]1[N:17]=[CH:18][C:19]([C:22]2[S:4][C:3]3[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=3[C:1](=[O:10])[N:23]=2)=[CH:20][CH:21]=1)([CH3:14])[CH3:13]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 21009Benzoic acid, 2-mercapto-, methyl esterHCID 229393206-Isopropoxynicotinonitrile

생성물 1

HCID 59750346HCID 59750346, 화합물수율 30%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of methyl thiosalicylate (1.85 g, 11.0 mmol), 2-isopropoxy-5-cyanopyridine (1.62 g, 10.0 mmol), triethylamine (1.80 ml, 12.9 mmol) and toluene (10 ml) was refluxed under nitrogen atmosphere for 30 hrs. The reaction mixture was concentrated. The residue was subjected to a silica gel column chromatography, eluted with ethyl acetate-hexane (2:1, v/v) and recrystallized from ethyl acetate-isopropylether to give the titled compound (0.89 g, 30%).

후처리

  1. temperaturewas refluxed under nitrogen atmosphere for 30 hrs
  2. concentrationThe reaction mixture was concentrated
  3. washeluted with ethyl acetate-hexane (2:1
  4. customv/v) and recrystallized from ethyl acetate-isopropylether

출처 및 근거

ORD 기록
ord-2a7eada100a643ffaea076fbd18ec4d5
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07399759B2

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