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Cesium carbonate → tert-Butyl (2-chloro-5-fluoropyridin-4-yl)carbamate

HRID 2171255
ノート
印刷プレビュー

反応式

HRID 2171255 の反応式
[C:1](=[O:8])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])[NH2:2].C(=O)([O-])[O-].[Cs+].[Cs+].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.[Cl:57][C:58]1[CH:63]=[C:62](I)[C:61]([F:65])=[CH:60][N:59]=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].O.C1(C)C=CC=CC=1>[Cl:57][C:58]1[CH:63]=[C:62]([NH:2][C:1](=[O:8])[O:3][C:4]([CH3:7])([CH3:6])[CH3:5])[C:61]([F:65])=[CH:60][N:59]=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 10796Cesium carbonateHCID 77922tert-Butyl carbamateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 248204952-Chloro-5-fluoro-4-iodopyridine

生成物 1

HCID 71741530tert-Butyl (2-chloro-5-fluoropyridin-4-yl)carbamate収率 79.8%

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

tert-Butyl carbamate (960 mg), cesium carbonate (5.06 g), Pd2(dba)3 (1.07 g), and Xantphos (1.35 g) were added to a toluene solution (40 ml) containing 2-chloro-5-fluoro-4-iodopyridine (2 g), followed by stirring at 100° C. for 3 hours. The reaction solution was adjusted to room temperature and water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layers were washed with saturated saline and dried over anhydrous sodium sulfate. The solvent was distilled away under reduced pressure and the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=9:1 to 4:1). A yellow oily matter of tert-butyl (2-chloro-5-fluoropyridin-4-yl)carbamate (1.53 g) was thus obtained.

後処理

  1. customwas adjusted to room temperature
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe organic layers were washed with saturated saline
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled away under reduced pressure
  6. customthe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=9:1 to 4:1)

出典と根拠

ORDレコード
ord-03c91063e62a4b90ac9c3ff8a207582d
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09051310B2

反応ノート

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