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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
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1,2-Diaminocyclohexane, trans- → N-[4-amino-3-(4-amino-3-methoxyphenyl)thieno[3,2-c]pyridin-7-yl]-2-pyrrolidin-1-ylacetamide triacetate salt

HRID 17231
ノート
印刷プレビュー

反応式

HRID 17231 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:12]3[C:13]([NH2:18])=[N:14][CH:15]=[C:16](I)[C:11]=3[S:10][CH:9]=2)=[CH:4][C:3]=1[O:19][CH3:20].[N:21]1([CH2:26][C:27]([NH2:29])=[O:28])[CH2:25][CH2:24][CH2:23][CH2:22]1.P([O-])([O-])([O-])=[O:31].[K+].[K+].[K+].[C@@H]1(N)CCCC[C@H]1N>[Cu]I.O1CCOCC1>[C:3]([OH:19])(=[O:28])[CH3:4].[C:27]([OH:28])(=[O:31])[CH3:26].[C:3]([OH:19])(=[O:28])[CH3:4].[NH2:18][C:13]1[C:12]2[C:8]([C:5]3[CH:6]=[CH:7][C:2]([NH2:1])=[C:3]([O:19][CH3:20])[CH:4]=3)=[CH:9][S:10][C:11]=2[C:16]([NH:29][C:27](=[O:28])[CH2:26][N:21]2[CH2:25][CH2:24][CH2:23][CH2:22]2)=[CH:15][N:14]=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 4

HCID 438061,2-Diaminocyclohexane, trans-HCID 62657Potassium Phosphate, TribasicHCID 134758251-PyrrolidineacetamideHCID 184507103-(4-Amino-3-methoxyphenyl)-7-iodothieno[3,2-c]pyridin-4-amine

生成物 1

HCID 18451403N-[4-amino-3-(4-amino-3-methoxyphenyl)thieno[3,2-c]pyridin-7-yl]-2-pyrrolidin-1-ylacetamide triacetate salt

試薬・触媒・溶媒 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 312751,4-Dioxane溶媒

反応条件

温度
110 °C

実験手順

A schlenck tube was charged with 3-(4-amino-3-methoxyphenyl)-7-iodothieno[3,2-c]pyridin-4-amine (199 mg, 0.5 mmol), 2-pyrrolidin-1-ylacetamide (0.6 mmol), copper(I) iodide (4.8 mg, 0.025 mmol), potassium phosphate (225 mg, 1.06 mmol). Evacuated under vacuum and back filled with nitrogen. trans-Cyclohexane-1,2-diamine (6.5 uL, 0.05 mmol) and dioxane (1 mL) was added. The reaction tube was sealed and heated at about 110° C. overnight. The solvent was removed and the crude product was purified by reverse phase preparative HPLC to give the title compound as the tri-acetate salt. LCMS (Conditions a): MH+=398.2, Rt=1.55 min. (154 mg, 45%)

後処理

  1. customEvacuated under vacuum
  2. additionback filled with nitrogen
  3. customThe reaction tube was sealed
  4. customThe solvent was removed
  5. customthe crude product was purified by reverse phase preparative HPLC

出典と根拠

ORDレコード
ord-a1656f847d5b4166abc0cb76fd0c498c
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07737160B2

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