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

HRID 499295ノート

反応式

HRID 499295 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-c22c970a9d16459db2bb457ea462f095
出典データセット
uspto-grants-2010_08
特許番号
US07767665B2

反応ノート

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