Triethylamine → HCID 59750374, 화합물

HRID 748140노트

반응식

HRID 748140 반응식
[C:1]([O:10]C)(=O)[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[SH:4].[N:12]1([C:18]2[CH:19]=[C:20]([CH:23]=[CH:24][N:25]=2)[C:21]#[N:22])[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[N:12]1([C:18]2[CH:19]=[C:20]([C:21]3[S:4][C:3]4[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=4[C:1](=[O:10])[N:22]=3)[CH:23]=[CH:24][N:25]=2)[CH2:13][CH2:14][O:15][CH2:16][CH2:17]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 21009Benzoic acid, 2-mercapto-, methyl esterHCID 146408562-(Morpholin-4-yl)pyridine-4-carbonitrile

생성물 1

HCID 59750374HCID 59750374, 화합물수율 25%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Methyl thiosalicylate (0.49 g, 2.9 mmol) and 2-morpholinylisonicotinonitrile (0.38 g, 2.0 mmol) were dissolved in toluene (2.0 ml), and triethylamine (0.48 ml, 3.4 mmol) was added thereto. The reaction mixture was refluxed for 14 hrs. After cooling, the precipitated crystals were collected by filtration and recrystallized from ethanol. The obtained crystals were recrystallized from ethyl acetate again to give the titled compound (0.16 g, 25%) as white crystals.

후처리

  1. temperatureThe reaction mixture was refluxed for 14 hrs
  2. temperatureAfter cooling
  3. filtrationthe precipitated crystals were collected by filtration
  4. customrecrystallized from ethanol
  5. customThe obtained crystals were recrystallized from ethyl acetate again

출처 및 근거

ORD 기록
ord-cc82206267b54091ae3a766ea1bd1a3a
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07399759B2

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