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

Dichloromethane → 2-Phenyl-5-(2-phenylpyrimidin-5-yl)oxazole

HRID 2096338
ノート
印刷プレビュー

反応式

HRID 2096338 の反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)Cl.Br[C:24]1[CH:25]=[N:26][C:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)=[N:28][CH:29]=1.[C:36]1([C:42]2[O:43][CH:44]=[CH:45][N:46]=2)[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1>C(=O)([O-])[O-].[Ag+2].C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].O>[C:36]1([C:42]2[O:43][C:44]([C:24]3[CH:25]=[N:26][C:27]([C:30]4[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=4)=[N:28][CH:29]=3)=[CH:45][N:46]=2)[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=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

8

反応物 4

HCID 6344DichloromethaneHCID 11776TriphenylphosphineHCID 5892802-Phenyl-1,3-oxazoleHCID 143877455-Bromo-2-phenylpyrimidine

生成物 1

HCID 592523852-Phenyl-5-(2-phenylpyrimidin-5-yl)oxazole収率 11%

試薬・触媒・溶媒 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 178418647HCID 178418647、化合物触媒
HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

Silver carbonate (317 mg, 1.15 mmol), triphenylphosphine (16 mg, 0.06 mmol) and Pd(dppf)Cl2.CH2Cl2 (24 mg, 5 mole %) were stirred together at room temperature under nitrogen. 5-Bromo-2-phenylpyrimidine (163 mg, 0.69 mmol) was added followed by 2-phenyl-oxazole (84 mg, 0.58 mmol; prepared according to Ohnmacht, S. A. et al., Chemical Communications, 2008, 1241-1243). Finally water (6 mL) was added and the mixture heated for 18 hours at 60° C. The mixture was cooled to room temperature and filtered through Celite washing with DCM and acetone. Purification by silica gel flash chromatography (100% DCM) through a 12-g Silicycle® flash silica cartridge gave title compound as light yellow solid (19 mg, 11% yield); Rf 0.68 with DCM; melting point 228-231° C.; 1H-NMR (300 MHz; DMSO-d6) δ 9.39 (s, 2H), 8.45 (dd, 2H), 8.17 (dd, 2H), 8.11 (s, 1H), 7.54-7.65 (m, 6H); MS (ESI+) m/z 300 (M+1), (ESI−) m/z 298 (M−1); H-PGDS FPBA IC50: 125 μM.

後処理

  1. customprepared
  2. temperatureThe mixture was cooled to room temperature
  3. filtrationfiltered through Celite
  4. washwashing with DCM and acetone
  5. customPurification by silica gel flash chromatography (100% DCM) through a 12-g Silicycle® flash silica cartridge

出典と根拠

ORDレコード
ord-e3a115a154104b76afe1340e426be5fe
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08450326B2

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