Triethylamine → 2-[5-(trifluoromethyl)-2-pyridyl]-4H-1,3-benzothiazine-4-one

HRID 748117ノート

反応式

HRID 748117 の反応式
[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][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][N:15]=1)#[N:13].C(N(CC)CC)C>C1(C)C=CC=CC=1>[F:22][C:20]([F:21])([F:23])[C:17]1[CH:18]=[CH:19][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)=[N:15][CH:16]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 21009Benzoic acid, 2-mercapto-, methyl esterHCID 15353725-(Trifluoromethyl)pyridine-2-carbonitrile

生成物 1

HCID 597500952-[5-(trifluoromethyl)-2-pyridyl]-4H-1,3-benzothiazine-4-one収率 23%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of methyl thiosalicylate (0.43 g, 2.6 mmol), 2-cyano-5-trifluoromethylpyridine (0.44 g, 2.6 mmol), triethylamine (0.60 ml, 3.8 mmol) and toluene (30 ml) was refluxed for 48 hrs as described in Example 1. The solvent was concentrated under reduced pressure. The residue was recrystallized from ethanol to give the titled compound (0.18 g, 23%) as crystals.

後処理

  1. temperaturewas refluxed for 48 hrs
  2. concentrationThe solvent was concentrated under reduced pressure
  3. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-39c597c224a14c209a14db298071cfd7
出典データセット
uspto-grants-2008_07
特許番号
US07399759B2

反応ノート

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