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Lithium Chloride → HCID 71240815、化合物

HRID 1774607
ノート
印刷プレビュー

反応式

HRID 1774607 の反応式
C[Sn](C)(C)[Sn](C)(C)C.[Cl-].[Li+].Cl[C:12]1[CH:17]=[C:16]([C:18]2[CH:23]=[CH:22][C:21]([O:24][CH:25]([CH3:27])[CH3:26])=[C:20]([Cl:28])[CH:19]=2)[N:15]=[CH:14][N:13]=1.[CH3:29][O:30][C:31]([CH:33]1[CH2:37][C:36](OS(C(F)(F)F)(=O)=O)=[CH:35][N:34]1[C:46]([O:48][C:49]([CH3:52])([CH3:51])[CH3:50])=[O:47])=[O:32]>C1COCC1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Pd]>[CH3:29][O:30][C:31]([CH:33]1[CH2:37][C:36]([C:12]2[CH:17]=[C:16]([C:18]3[CH:23]=[CH:22][C:21]([O:24][CH:25]([CH3:27])[CH3:26])=[C:20]([Cl:28])[CH:19]=3)[N:15]=[CH:14][N:13]=2)=[CH:35][N:34]1[C:46]([O:48][C:49]([CH3:52])([CH3:51])[CH3:50])=[O:47])=[O:32]
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

7

反応物 4

HCID 433294Lithium ChlorideHCID 85161366HCID 85161366、化合物HCID 89396901HCID 89396901、化合物HCID 178477788HCID 178477788、化合物

生成物 1

HCID 71240815HCID 71240815、化合物収率 9%

試薬・触媒・溶媒 2

HCID 11979704
Tetrakis(triphenylphosphine)palladium
触媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

Hexamethyldistannane (5.6 ml, 2.7 mmol) and lithium chloride (0.34 g, 7.8 mmol) were added sequentially in one portion to a stirred solution of, 4-chloro-6-(3-chloro-4-isopropoxy-phenyl)-pyrimidine (0.75 g, 2.7 mmol) and 4-trifluoromethanesulfonyloxy-2,3-dihydro-pyrrole-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (1.0 g, 2.7 mmol) in THF (40 ml). The mixture was degassed with nitrogen for 5 minutes, after which time palladium tetrakis(triphenylphosphine) (0.31 g, 0.26 mmol) was added in one portion, the mixture was then heated to 70° C. and stirred at this temperature for 16 hours under a nitrogen atmosphere. After this time the reaction mixture was cooled to room temperature and partitioned between ethyl acetate (200 ml) and saturated potassium fluoride (50 ml). The organic layer was separated, washed sequentially with water (100 ml) then brine (100 ml) before being dried (MgSO4), filtered and concentrated. The resulting red gum was purified by flash column chromatography (elution: 80% EtOAc, 20% Heptane) to give the title compound (0.1 g, 9% yield) as a colourless oil. Tr=2.69 min m/z (ES+) (M+H+) 474.

後処理

  1. customThe mixture was degassed with nitrogen for 5 minutes
  2. temperatureAfter this time the reaction mixture was cooled to room temperature
  3. custompartitioned between ethyl acetate (200 ml) and saturated potassium fluoride (50 ml)
  4. customThe organic layer was separated
  5. washwashed sequentially with water (100 ml)
  6. dry with materialbrine (100 ml) before being dried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe resulting red gum was purified by flash column chromatography (elution: 80% EtOAc, 20% Heptane)

出典と根拠

ORDレコード
ord-bda38543c00c42d784b7db45bbb755c1
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09260422B2

反応ノート

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