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Pyridine → 2-[5-(3,5-Bistrifluoromethylpyrazol-1-ylmethyl)-2-(3-chloropyridin-2-yl)-2H-pyrazol-3-yl]-6-chloro-8-methylbenzo[d][1,3]oxazin-4-one

HRID 1842538
ノート
印刷プレビュー

反応式

HRID 1842538 の反応式
CS(Cl)(=O)=O.[F:6][C:7]([F:34])([F:33])[C:8]1[CH:12]=[C:11]([C:13]([F:16])([F:15])[F:14])[N:10]([CH2:17][C:18]2[CH:19]=[C:20]([C:30](O)=[O:31])[N:21]([C:23]3[C:28]([Cl:29])=[CH:27][CH:26]=[CH:25][N:24]=3)[N:22]=2)[N:9]=1.N1C=CC=CC=1.[NH2:41][C:42]1[C:51]([CH3:52])=[CH:50][C:49]([Cl:53])=[CH:48][C:43]=1[C:44](NC)=[O:45]>C(#N)C>[F:34][C:7]([F:6])([F:33])[C:8]1[CH:12]=[C:11]([C:13]([F:16])([F:15])[F:14])[N:10]([CH2:17][C:18]2[CH:19]=[C:20]([C:30]3[O:31][C:44](=[O:45])[C:43]4[CH:48]=[C:49]([Cl:53])[CH:50]=[C:51]([CH3:52])[C:42]=4[N:41]=3)[N:21]([C:23]3[C:28]([Cl:29])=[CH:27][CH:26]=[CH:25][N:24]=3)[N:22]=2)[N:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1049Pyridine2 回HCID 31297Methanesulfonyl chloride2 回HCID 250682512-Amino-5-Chloro-N,3-DimethylbenzamideHCID 866385275-(3,5-bistrifluoromethylpyrazol-1-ylmethyl)-2-(3-chloropyridin-2-yl)-2H-pyrazole-3-carboxylic acid

生成物 1

HCID 591730282-[5-(3,5-Bistrifluoromethylpyrazol-1-ylmethyl)-2-(3-chloropyridin-2-yl)-2H-pyrazol-3-yl]-6-chloro-8-methylbenzo[d][1,3]oxazin-4-one

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒3 回

実験手順

Under argon 0.12 ml (1.60 mmol) of methanesulphonyl chloride in 3 ml of acetonitrile are cooled to 0° C. and subsequently a solution of 540 mg (1.228 mmol) of 5-(3,5-bistrifluoromethylpyrazol-1-ylmethyl)-2-(3-chloropyridin-2-yl)-2H-pyrazole-3-carboxylic acid in 0.17 ml (2.09 mmol) of pyridine and 6 ml of acetonitrile is added dropwise. The mixture is stirred at this temperature for 15 minutes and then a solution of 228 mg (1.228 mmol) of 2-amino-5-chloro-3,N-dimethylbenzamide in 0.35 ml (4.30 mmol) of pyridine and 6 ml of acetonitrile is added. After a further 15 minutes at 0° C. the mixture is admixed with 0.12 ml (1.60 mmol) of methanesulphonyl chloride and warmed slowly to room temperature overnight. The solvent is removed in vacuo, 15 ml of water are added and the crystals formed are filtered off with suction.

後処理

  1. customThe solvent is removed in vacuo, 15 ml of water
  2. additionare added
  3. customthe crystals formed
  4. filtrationare filtered off with suction

出典と根拠

ORDレコード
ord-96a6e6f81dc04e14bda22b6891e4cd1d
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946236B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート