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Sodium Carbonate → HCID 59765138、化合物

HRID 536206
ノート
印刷プレビュー

反応式

HRID 536206 の反応式
[Cl:1][C:2]1[C:7](I)=[C:6]([NH2:9])[CH:5]=[CH:4][N:3]=1.[Cl-].[Li+].C(=O)([O-])[O-].[Na+].[Na+].[CH3:18][O:19][C:20]1[CH:21]=[C:22]([C:26]#[C:27][Si:28]([CH3:31])([CH3:30])[CH3:29])[CH:23]=[CH:24][CH:25]=1>CN(C=O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].O>[Cl:1][C:2]1[C:7]2[C:26]([C:22]3[CH:23]=[CH:24][CH:25]=[C:20]([O:19][CH3:18])[CH:21]=3)=[C:27]([Si:28]([CH3:31])([CH3:29])[CH3:30])[NH:9][C:6]=2[CH:5]=[CH:4][N:3]=1
参加物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 10340Sodium CarbonateHCID 433294Lithium ChlorideHCID 4407093(3-Methoxyphenylethynyl)trimethylsilaneHCID 242292082-Chloro-3-iodopyridin-4-amine

生成物 1

HCID 59765138HCID 59765138、化合物

試薬・触媒・溶媒 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

実験手順

7.6 g (30 mmol) of 2-chloro-3-iodopyridin-4-ylamine from Example B1, 1.7 g (41 mmol) of lithium chloride and 15.9 g (120 mmol) of sodium carbonate are dissolved in 100 ml of DMF, and 8 g (39 mmol) of commercial (3-methoxyphenyl)ethynyltrimethylsilane and 4.9 g (6 mmol) of commercial Pd(dppf)2Cl2*H2Cl2 are added at 100° C. under nitrogen. The mixture is stirred at the temperature indicated for 12 h and subsequently poured at room temperature (RT) into water and extracted with ethyl acetate. The organic phase is concentrated and purified by chromatography over silica gel. The combined product fractions (5.3 g; 53%; pale-brown oil) are used for the subsequent reaction.

後処理

  1. extractionextracted with ethyl acetate
  2. concentrationThe organic phase is concentrated
  3. custompurified by chromatography over silica gel
  4. customThe combined product fractions (5.3 g; 53%; pale-brown oil) are used for the subsequent reaction

出典と根拠

ORDレコード
ord-7d482365f65d4cef9d1d7cbe1af86923
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08859581B2

反応ノート

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