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1,2-Dimethoxyethane → HCID 73877973、化合物

HRID 1612045
ノート
印刷プレビュー

反応式

HRID 1612045 の反応式
Br[C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([F:9])[C:3]=1[NH:10][C:11]([C:13]1[C:14]([CH3:20])=[N:15][N:16]([CH3:19])[C:17]=1[F:18])=[O:12].[CH3:21][O:22][N:23]=[CH:24][C:25]1[CH:30]=[CH:29][C:28](B(O)O)=[CH:27][CH:26]=1.COCCOC.C(=O)([O-])[O-].[Na+].[Na+]>O.[Pd].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>[F:9][C:4]1[C:3]([NH:10][C:11]([C:13]2[C:14]([CH3:20])=[N:15][N:16]([CH3:19])[C:17]=2[F:18])=[O:12])=[C:2]([C:28]2[CH:29]=[CH:30][C:25]([CH:24]=[N:23][O:22][CH3:21])=[CH:26][CH:27]=2)[CH:7]=[C:6]([F:8])[CH:5]=1
参加物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 80711,2-DimethoxyethaneHCID 10340Sodium CarbonateHCID 22252919HCID 22252919、化合物HCID 714471054-[(Methoxyimino)methyl]phenylboronic acid

生成物 1

HCID 73877973HCID 73877973、化合物収率 49.7%

試薬・触媒・溶媒 2

HCID 11979704
Tetrakis(triphenylphosphine)palladium
触媒
HCID 962Water溶媒2 回

実験手順

At room temperature, a mixture of 0.35 g (0.001 mol) of N-(2-bromo-4,6-difluorophenyl)-5-fluoro-1,3-dimethyl-1H-pyrazole-4-carboxamide, 0.06 g (0.00005 mol) of tetrakis-(triphenylphosphine)-palladium, 0.32 g (0.0018 mol) of 4-[(methoxyimino)methyl]phenylboronic acid and 10 ml of 1,2-dimethoxyethane is admixed with a solution of 0.5 g (0.0047 mol) of sodium carbonate in 3 ml of water. The reaction mixture is then heated to reflux temperature and kept at this temperature for 15 h. For work-up, the reaction mixture is stirred into 200 ml of water. The resulting precipitate is filtered off with suction and dried. The residue that remains is chromatographed on silica gel using the mobile phase cyclohexane:ethyl acetate=1:1. Concentration of the eluate gives 0.20 g (48% of theory) of N-{3,5-difluoro-4′-[(methoxyimino)methyl]-1,1′-biphenyl-2-yl}-5-fluoro-1,3-dimethyl-1H-pyrazole-4-carboxamide in the form of a solid of melting point 164 to 167° C.

後処理

  1. temperatureThe reaction mixture is then heated
  2. temperatureto reflux temperature
  3. filtrationThe resulting precipitate is filtered off with suction
  4. customdried
  5. customThe residue that remains is chromatographed on silica gel using the mobile phase cyclohexane

出典と根拠

ORDレコード
ord-1892704222334603a507681d7dd6e44d
出典データセット
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06992098B2

反応ノート

読み込み中…

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