ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Lithium Hydroxide → HCID 67361802、化合物

HRID 1183175
ノート
印刷プレビュー

反応式

HRID 1183175 の反応式
COC(C1C=C(O)N(C2C=CC=CC=2F)N=1)=O.C(=O)([O-])[O-].[Cs+].[Cs+].BrCC1C=CC=CC=1C#N.C[O:35][C:36]([C:38]1[CH:42]=[C:41]([O:43][CH2:44][C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][C:46]=2[C:51]#[N:52])[N:40]([C:53]2[CH:58]=[CH:57][CH:56]=[CH:55][C:54]=2[F:59])[N:39]=1)=[O:37].[OH-].[Li+]>CN(C=O)C.C1COCC1.O>[C:51]([C:46]1[CH:47]=[CH:48][CH:49]=[CH:50][C:45]=1[CH2:44][O:43][C:41]1[N:40]([C:53]2[CH:58]=[CH:57][CH:56]=[CH:55][C:54]=2[F:59])[N:39]=[C:38]([C:36]([OH:37])=[O:35])[CH:42]=1)#[N:52]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 3939Lithium HydroxideHCID 10796Cesium carbonateHCID 895992-(Bromomethyl)benzonitrileHCID 71257690HCID 71257690、化合物HCID 178498589HCID 178498589、化合物

生成物 1

HCID 67361802HCID 67361802、化合物収率 86.4%

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

1-(2-Fluoro-phenyl)-5-hydroxy-1H-pyrazole-3-carboxylic acid methyl ester (200 mg, 0.847 mmol) were dissolved in 5 ml of DMF and cesium carbonate (552 mg, 1.7 mmol) and 2-bromomethyl-benzonitrile (166 mg, 0.85 mmol) were added. The mixture was stirred for 5 h at 60° C., filtrated and the solvent was removed in vacuo. The obtained residue of crude 5-(2-cyano-benzyloxy)-1-(2-fluoro-phenyl)-1H-pyrazole-3-carboxylic acid methyl ester (235 mg, 79%) was dissolved in a mixture of THF, MOH and water (3 ml each), lithium hydroxide (64.1 mg, 2.7 mmol) was added, and the mixture was stirred overnight at room temperature. After evaporation of the solvent the residue was subjected to column chromatography (silica gel, DCM/MOH 9:1) to give 195 mg (86%) of the title compound.

後処理

  1. filtrationfiltrated
  2. customthe solvent was removed in vacuo
  3. additionwas added
  4. stirringthe mixture was stirred overnight at room temperature
  5. customAfter evaporation of the solvent the residue

出典と根拠

ORDレコード
ord-0cd5b384b5864f668dd840a368fa0883
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08664257B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート