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 → (1R,2S)-(1-(4-fluorophenyl)-1H-indazol-5-yloxy)-1-phenylpentan-2-amine

HRID 13102
ノート
印刷プレビュー

反応式

HRID 13102 の反応式
Cl.[NH2:2][C@@H:3]([CH2:12][CH2:13][CH3:14])[C@@H:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[OH:5].[Ar].[F:16][C:17]1[CH:22]=[CH:21][C:20]([N:23]2[C:31]3[C:26](=[CH:27][C:28](I)=[CH:29][CH:30]=3)[CH:25]=[N:24]2)=[CH:19][CH:18]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>C(#N)CCC.[Cu]I>[F:16][C:17]1[CH:18]=[CH:19][C:20]([N:23]2[C:31]3[C:26](=[CH:27][C:28]([O:5][C@H:4]([C:6]4[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=4)[C@@H:3]([NH2:2])[CH2:12][CH2:13][CH3:14])=[CH:29][CH:30]=3)[CH:25]=[N:24]2)=[CH:21][CH:22]=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

6

反応物 3

HCID 10796Cesium carbonateHCID 592511281-(4-fluorophenyl)-5-iodo-1H-indazoleHCID 86623008argon (1R,2S)-2-amino-1-phenylpentan-1-ol hydrochloride

生成物 1

HCID 59339774(1R,2S)-(1-(4-fluorophenyl)-1H-indazol-5-yloxy)-1-phenylpentan-2-amine

試薬・触媒・溶媒 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 8008Butyronitrile溶媒

反応条件

温度
125 °C

実験手順

In a vial under argon (1R,2S)-2-amino-1-phenylpentan-1-ol hydrochloride (91b, 46 mg, 0.21 mmol), 1-(4-fluorophenyl)-5-iodo-1H-indazole (87 mg, 0.26 mmol), copper(I)iodide (8.12 mg, 0.04 mmol) and cesium carbonate (278 mg, 0.85 mmol) were mixed in butyronitrile (0.6 mL). The vial was sealed and heated to 125° C. for 16 h. The mixture was filtered through celite. The celite was washed with ethyl acetate. The collected organic phases were evaporated and the crude product was purified by preparative HPLC. The pure fractions were collected, ethyl acetate and a saturated sodium carbonate were added and the mixture was shaken. The organic layer was separated and the water layer was washed twice with ethyl acetate. The combined organic layers were dried over sodium sulphate and finally evaporated to give the pure product.

後処理

  1. customThe vial was sealed
  2. filtrationThe mixture was filtered through celite
  3. washThe celite was washed with ethyl acetate
  4. customThe collected organic phases were evaporated
  5. customthe crude product was purified by preparative HPLC
  6. customThe pure fractions were collected
  7. additionethyl acetate and a saturated sodium carbonate were added
  8. customThe organic layer was separated
  9. washthe water layer was washed twice with ethyl acetate
  10. dry with materialThe combined organic layers were dried over sodium sulphate
  11. customfinally evaporated
  12. customto give the pure product

出典と根拠

ORDレコード
ord-de25f8a7ec5b4322bcb8649f1d574484
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07728030B2

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