1,2-Dichloroethane → HCID 178470495、化合物

HRID 20309

反応式

HRID 20309 の反応式
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4]([OH:6])=O.[CH2:12]([O:14][C:15]([C:17]1[C:21]([NH2:22])=[CH:20][NH:19][N:18]=1)=[O:16])[CH3:13].C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C.O>[CH2:12]([O:14][C:15]([C:17]1[C:21]([NH:22][C:4](=[O:6])[C:3]2[C:7]([F:11])=[CH:8][CH:9]=[CH:10][C:2]=2[F:1])=[CH:20][NH:19][N:18]=1)=[O:16])[CH3:13]

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 97962,6-Difluorobenzoic acidHCID 757711-HydroxybenzotriazoleHCID 178470494HCID 178470494、化合物

生成物 1

HCID 178470495HCID 178470495、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2,6-difluorobenzoic acid (6.32 g, 40.0 mmol), 4-amino-1H-pyrazole-3-carboxylic acid ethyl ester (5.96 g, 38.4 mmol), EDC (8.83 g, 46.1 mmol) and HOBt (6.23 g, 46.1 mmol) in DMF (100 ml) was stirred at ambient temperature for 6 h. The mixture was reduced in vacuo, water added and the solid formed collected by filtration and air-dried to give 4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid ethyl ester as the major component of a mixture (15.3 g). (LC/MS: Rt 3.11, [M+H]+ 295.99).

後処理

  1. additionadded
  2. customthe solid formed
  3. filtrationcollected by filtration
  4. customair-dried

出典と根拠

ORDレコード
ord-b3a36254da974d729f01f69d5c130ffe
出典データセット
uspto-grants-2010_06
特許番号
US07745638B2

関連ノート

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