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Diethylethanolamine → HCID 58879980、化合物

HRID 1361419
ノート
印刷プレビュー

反応式

HRID 1361419 の反応式
[C:1]([C:4]1[CH:9]=[C:8]([O:10][C:11]2[CH:19]=[CH:18][C:14]([C:15]([OH:17])=O)=[CH:13][C:12]=2[F:20])[CH:7]=[CH:6][N:5]=1)(=[O:3])[NH2:2].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:45][C:46]1[C:47](=[O:59])[N:48]([C:52]2[CH:57]=[CH:56][C:55]([F:58])=[CH:54][CH:53]=2)[CH:49]=[CH:50][CH:51]=1.CCN(CCO)CC>CN(C=O)C.CO>[F:20][C:12]1[CH:13]=[C:14]([C:15](=[O:17])[NH:45][C:46]2[C:47](=[O:59])[N:48]([C:52]3[CH:57]=[CH:56][C:55]([F:58])=[CH:54][CH:53]=3)[CH:49]=[CH:50][CH:51]=2)[CH:18]=[CH:19][C:11]=1[O:10][C:8]1[CH:7]=[CH:6][N:5]=[C:4]([C:1]([NH2:2])=[O:3])[CH:9]=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

7

反応物 4

HCID 7497DiethylethanolamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 58879956HCID 58879956、化合物HCID 588799723-amino-1-(4-fluorophenyl)pyridin-2(1H)-one

生成物 1

HCID 58879980HCID 58879980、化合物収率 57%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

To a solution of 4-(2-carbamoylpyridin-4-yloxy)-3-fluorobenzoic acid (0.3 mmol, 83 mg) in DMF (2 mL), were added HATU (Perspective Biosystems, 0.45 mmol, 171 mg), 3-amino-1-(4-fluorophenyl)pyridin-2(1H)-one (0.3 mmol, 61.2 mg) and DEEA (Aldrich, 0.2 mL). The reaction mixture were heated at 50° C. for 5 h. After cooling to room temperature, 5 mL of methanol was added. The product was purified by preparative HPLC. The desired fractions were combined, neutralized to pH 7-8 with aq. K2HPO4, and concentrated in vacuo. The precipitate that formed was collected by filtration, rinsed with water, and dried under vacuum to give the desired product (78 mg, 57% yield). MS(ESf+) m/z 463.25 (M+H)+.

後処理

  1. temperatureAfter cooling to room temperature
  2. customThe product was purified by preparative HPLC
  3. concentrationconcentrated in vacuo
  4. customThe precipitate that formed
  5. filtrationwas collected by filtration
  6. washrinsed with water
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-ecdfdf6fdb3e451dbf7821a3bb60bcd1
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07880004B2

反応ノート

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