Selectfluor → 4-amino-8-(cyclopentyloxy)-3-fluoro-7-methoxy-2H-chromen-2-one

HRID 20642

反応式

HRID 20642 の反応式
[NH2:1][C:2]1[C:11]2[C:6](=[C:7]([O:14][CH:15]3[CH2:19][CH2:18][CH2:17][CH2:16]3)[C:8]([O:12][CH3:13])=[CH:9][CH:10]=2)[O:5][C:4](=[O:20])[CH:3]=1.[B-](F)(F)(F)[F:22].[B-](F)(F)(F)F.C1[N+]2(CCl)CC[N+](F)(CC2)C1>C(#N)C>[NH2:1][C:2]1[C:11]2[C:6](=[C:7]([O:14][CH:15]3[CH2:19][CH2:18][CH2:17][CH2:16]3)[C:8]([O:12][CH3:13])=[CH:9][CH:10]=2)[O:5][C:4](=[O:20])[C:3]=1[F:22]

参加物

4

反応物 2

HCID 2724933SelectfluorHCID 771747934-amino-8-(cyclopentyloxy)-7-methoxy-2H-chromen-2-one

生成物 1

HCID 866181344-amino-8-(cyclopentyloxy)-3-fluoro-7-methoxy-2H-chromen-2-one

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 4-amino-8-(cyclopentyloxy)-7-methoxy-2H-chromen-2-one (100 mg, 0.36 mmol, Example 3, Step 1), Selectfluor (160 mg, 0.45 mmol), and acetonitrile (1.5 mL) were stirred vigorously for 18 h, concentrated, and then purified by silica gel chromatography (7:3→1:4; hexanes:ethyl acetate) to give 4-amino-8-(cyclopentyloxy)-3-fluoro-7-methoxy-2H-chromen-2-one: MS (ESI): 294.0.

後処理

  1. concentrationconcentrated
  2. custompurified by silica gel chromatography (7:3→1:4; hexanes:ethyl acetate)

出典と根拠

ORDレコード
ord-1f2b2ae8e5f1496aafb24688b567536b
出典データセット
uspto-grants-2010_06
特許番号
US07745646B2

関連ノート

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