Triethylamine → 2-[6-(Isoamylthio)-2-pyridyl]-4H-1,3-benzothiazine-4-one

HRID 748196노트

반응식

HRID 748196 반응식
[C:1]([O:10]C)(=O)[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[SH:4].[C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([S:20][CH2:21][CH2:22][CH:23]([CH3:25])[CH3:24])[N:15]=1)#[N:13].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH2:21]([S:20][C:16]1[N:15]=[C:14]([C:12]2[S:4][C:3]3[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=3[C:1](=[O:10])[N:13]=2)[CH:19]=[CH:18][CH:17]=1)[CH2:22][CH:23]([CH3:25])[CH3:24]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 21009Benzoic acid, 2-mercapto-, methyl esterHCID 229393372-Cyano-6-isopentylthiopyridine

생성물 1

HCID 229395222-[6-(Isoamylthio)-2-pyridyl]-4H-1,3-benzothiazine-4-one수율 26%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of methyl thiosalicylate (1.21 g, 7.2 mmol), 2-cyano-6-isopentylthiopyridine (1.48 g, 7.2 mmol), triethylamine (1.5 ml, 10.8 mmol) and toluene (30 ml) was refluxed for 48 hrs. The reaction mixture was concentrated under reduced pressure to give the precipitated crystals, which were recrystallized from ethyl acetate-hexane to give the titled compound (0.64 g, 26%).

후처리

  1. temperaturewas refluxed for 48 hrs
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customto give the precipitated crystals, which
  4. customwere recrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-ccde31d0517c443ba5f5babb161013ae
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07399759B2

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