Water → HCID 178473464、化合物

HRID 489948

反応式

HRID 489948 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:12]([C:13]3[CH:18]=[CH:17][N:16]=[C:15]([NH2:19])[N:14]=3)=[CH:11][NH:10][N:9]=2)=[CH:4][CH:3]=1.C1C=NC(NS(C2C=CC(N)=CC=2)(=O)=O)=NC=1.Cl[C:38]([O:40][CH2:41][CH3:42])=[O:39].O>N1C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:12]([C:13]3[CH:18]=[CH:17][N:16]=[C:15]([NH:19][C:38](=[O:39])[O:40][CH2:41][CH3:42])[N:14]=3)=[CH:11][NH:10][N:9]=2)=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 5215SulfadiazineHCID 10928Ethyl chloroformateHCID 1785083854-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyrimidinamine

生成物 1

HCID 178473464HCID 178473464、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a suspension of 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyrimidinamine prepared in accordance with Example A-306 (0.26 g, 0.001 mol) in 5 mL of pyridine was added ethyl chloroformate dropwise. After the addition, the clear solution was stirred at room temperature for 6 hours. Water was added and the aqueous phase was extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate and filtered. The filtrate was concentrated and the crude was trituated with ether to give 0.15 g of product, ethyl (4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyrimidinyl]carbamate, as a white solid (46% yield), mp: 163-165° C.; Anal. Calc'd for C16H14FN5O2: C, 58.71; H, 4.31; N, 21.04. Found: C, 59.22; H, 4.51; N, 21.66.

後処理

  1. additionAfter the addition
  2. extractionthe aqueous phase was extracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-8bb23441900d4d5c8aa7ef7af4b00511
出典データセット
uspto-grants-2005_12
特許番号
US06979686B1

関連ノート

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