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

HRID 499379노트

반응식

HRID 499379 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-423a5a05fe124b24b8461e5885033767
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07767665B2

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