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

Water → HCID 11579342、化合物

HRID 576705
ノート
印刷プレビュー

反応式

HRID 576705 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:8]=[CH:7][N:6]=[C:5]([C:9]([OH:11])=[O:10])[N:4]=1.[CH3:14][Si](C=[N+]=[N-])(C)C.O>C1COCC1.CO.CC(O)=O>[F:13][C:2]([F:1])([F:12])[C:3]1[CH:8]=[CH:7][N:6]=[C:5]([C:9]([O:11][CH3:14])=[O:10])[N:4]=1
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

7

反応物 3

HCID 962WaterHCID 167693TrimethylsilyldiazomethaneHCID 253241464-(Trifluoromethyl)pyrimidine-2-carboxylic acid

生成物 1

HCID 11579342HCID 11579342、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid触媒HCID 887Methanol溶媒
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
0 °C

実験手順

4-(trifluoromethyl)pyrimidine-2-carboxylic acid (500 mg, 2.6 mmol) was dissolved in a mixture of 1 mL of THF and 300 μL of MeOH and cooled to 0° C. Trimethylsilyldiazomethane (2M in ether, 2.6 mL, 5.2 mmol) was added dropwise. The solution was stirred for 2 hours at 0° C., then 1 hour at rt. A few drops of AcOH were added, followed by water. The aqueous solution was extracted three times with EtOAc. The combined organic layers were dried (Na2SO4), filtered, and concentrated to give an oil which was used without further purification. MS (ESI): mass calcd. for C7H5F3N2O2, 206.0; m/z found, 207.0 [M+H]+. 1H NMR (400 MHz, CDCl3) δ 9.24 (d, J=5.0 Hz, 1H), 7.87 (d, J=5.0 Hz, 1H), 4.10 (s, 3H).

後処理

  1. custom1 hour
  2. customat rt
  3. extractionThe aqueous solution was extracted three times with EtOAc
  4. dry with materialThe combined organic layers were dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto give an oil which
  8. customwas used without further purification

出典と根拠

ORDレコード
ord-2ecd3e9a2eb5413a89c3927d256f4a34
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09040534B2

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