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

Cesium carbonate → HCID 42629845、化合物

HRID 1880616
ノート
印刷プレビュー

反応式

HRID 1880616 の反応式
Br.[Cl:2][C:3]1[C:12]([OH:13])=[C:11]([OH:14])[C:10]([Cl:15])=[C:9]2[C:4]=1[CH2:5][CH2:6][NH:7][CH2:8]2.[CH3:16][C:17]1[C:22](/[CH:23]=[CH:24]/[C:25](O)=[O:26])=[CH:21][CH:20]=[C:19]([C:28]([F:31])([F:30])[F:29])[N:18]=1.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C1C=CN=CC=1)C.CN(C=O)C.O>[Cl:2][C:3]1[C:12]([OH:13])=[C:11]([OH:14])[C:10]([Cl:15])=[C:9]2[C:4]=1[CH2:5][CH2:6][N:7]([C:25](=[O:26])/[CH:24]=[CH:23]/[C:22]1[C:17]([CH3:16])=[N:18][C:19]([C:28]([F:29])([F:30])[F:31])=[CH:20][CH:21]=1)[CH2:8]2
参加物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 10796Cesium carbonateHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 57808084HCID 57808084、化合物HCID 685081725,8-Dichloro-1,2,3,4-tetrahydroisoquinoline-6,7-diol hydrobromide

生成物 1

HCID 42629845HCID 42629845、化合物
収率 11%

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

5,8-Dichloro-1,2,3,4-tetrahydroisoquinoline-6,7-diol hydro bromide (183 mg, 0.58 mmol), (E)-3-(2-methyl-6-(trifluoromethyl)pyridin-3-yl)acrylic acid (140 mg, 0.64 mmol), EDC.HCl (167 mg, 0.87 mmol), HOBt (89 mg, 0.58 mmol), DMAP (147 mg, 1.2 mmol) and Cs2CO3 (391 mg, 1.2 mmol) were suspended in DMF (15 mL) and stirred at rt for 12 h. The reaction mixture was then diluted with water (30 mL) and extracted with EtOAc (3×30 mL). Combined organics were washed with NaHCO3 (2×30 mL, sat. aq.), water (3×30 mL) and brine and dried (MgSO4). After filtration and evaporation the residue was purified by column chromatography (SiO2, CH2Cl2:MeOH 95:5) and was then further purified by size exclusion chromatography (sephadex, CHCl3:MeOH 1:1) to give the title compound (28 mg, 63 μmol, 11%) as a yellow solid.

後処理

  1. extractionextracted with EtOAc (3×30 mL)
  2. washCombined organics were washed with NaHCO3 (2×30 mL, sat. aq.), water (3×30 mL) and brine
  3. dry with materialdried (MgSO4)
  4. filtrationAfter filtration and evaporation the residue
  5. customwas purified by column chromatography (SiO2, CH2Cl2:MeOH 95:5)
  6. customwas then further purified by size exclusion chromatography (sephadex, CHCl3:MeOH 1:1)

出典と根拠

ORDレコード
ord-8055999995444c849488fc6fc6192328
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08318768B2

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