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2-Fluoro-5-iodopyridine → HCID 16748705、化合物

HRID 914753
ノート
印刷プレビュー

反応式

HRID 914753 の反応式
[C@H:1]12[CH2:7][C@H:4]([NH:5][CH2:6]1)[CH2:3][N:2]2[C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9].[F:15][C:16]1[CH:21]=[CH:20][C:19](I)=[CH:18][N:17]=1.COC1C=CC2C(=CC=CC=2)C=1C1C2C(=CC=CC=2)C=CC=1P(C1C=CC=CC=1)C1C=CC=CC=1.CC(C)([O-])C.[Na+]>C1(C)C=CC=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C(OCC)C>[F:15][C:16]1[N:17]=[CH:18][C:19]([N:5]2[CH2:6][C@@H:1]3[CH2:7][C@H:4]2[CH2:3][N:2]3[C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])=[CH:20][CH:21]=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 27831792-Fluoro-5-iodopyridineHCID 4190002(2'-Methoxy-1,1'-binaphthalen-2-yl)(diphenyl)phosphineHCID 11521263(1S,4S)-2-Boc-2,5-diazabicyclo[2.2.1]heptaneHCID 23676156Sodium t-butoxide

生成物 1

HCID 16748705HCID 16748705、化合物収率 32.1%

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 1140Toluene溶媒
HCID 3283Diethyl Ether溶媒

反応条件

温度
80 °C

実験手順

tert-Butyl (1S,4S)-2,5-diazabicyclo[2.2.1]heptane-2-carboxylate (0.300 g, 1.01 mmol), prepared as described in (J. Med. Chem., (1988) 31, 1598-1611), in anhydrous toluene (30 ml) was treated with 2-fluoro-5-iodopyridine (0.34 g, 1.52 mmol), available as described in (U.S. Pat. No. 5,733,912), Pd2(dba)3 (0.028 g, 0.03 mmol), (S)-(−)-2-(diphenylphosphino)-2′-methoxy-1,1′-binaphthyl (0.028 g, 0.06 mmol), available from Strem Chemicals, and sodium tert-butoxide (0.248 g, 2.58 mmol). The reaction mixture was heated at 80° C. for 5 hours. The reaction mixture was poured into diethyl ether (100 mL), washed with brine (100 ml), dried (MgSO4), and concentrated under reduced pressure. The residue was purified by chromatography on SiO2 (3% MeOH/CH2Cl2) to provide the title compound (0.095 g, 21% yield) as a yellow oil. MS (DCI/NH3) m/z 276 (M+H)+.

後処理

  1. washwashed with brine (100 ml)
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by chromatography on SiO2 (3% MeOH/CH2Cl2)

出典と根拠

ORDレコード
ord-c3c6d36e5c3c445fa8d85a05b0fad08c
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07265115B2

反応ノート

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