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1,2-Dichloroethane → HCID 67496994、化合物

HRID 1628339
ノート
印刷プレビュー

反応式

HRID 1628339 の反応式
[CH3:1][N:2]1[C:6]([NH2:7])=[CH:5][C:4]([C:8]2[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=2)=[N:3]1.[CH3:14][C:15]([O:18][C:19]([NH:21][C@H:22]([C:31](O)=[O:32])[CH2:23][C:24]1[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=1)=[O:20])([CH3:17])[CH3:16].C(Cl)CCl>N1C=CC=CC=1>[F:30][C:27]1[CH:28]=[CH:29][C:24]([CH2:23][C@H:22]([NH:21][C:19](=[O:20])[O:18][C:15]([CH3:16])([CH3:14])[CH3:17])[C:31]([NH:7][C:6]2[N:2]([CH3:1])[N:3]=[C:4]([C:8]3[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=3)[CH:5]=2)=[O:32])=[CH:25][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 111,2-DichloroethaneHCID 7020910N-(tert-Butoxycarbonyl)-4-fluoro-L-phenylalanineHCID 337835201-Methyl-3-(pyridin-4-yl)-1H-pyrazol-5-amine

生成物 1

HCID 67496994HCID 67496994、化合物収率 99.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a 100 ml flask was added 1-methyl-3-(pyridin-4-yl)-1H-pyrazol-5-amine 17.B (540 mg, 3.10 mmole), Boc-L-4-fluorophenylalanine (970 mg, 3.41 mmole), EDC (710 mg, 3.72 mmole), and 10 ml of pyridine. The reaction was stirred at room temperature for 5.5 hours at which time the solvent was removed by rotary evaporation. The residue was suspended in ethyl acetate, and washed successively with saturated sodium bicarbonate, water and brine. The organic layer was dried over anhydrous sodium sulfate, and concentrated in vacuo. The crude product was purified by silica gel chromatography to give 103.1.A (1.35 g, 99% yield) as colorless amorphous.

後処理

  1. customwas removed by rotary evaporation
  2. washwashed successively with saturated sodium bicarbonate, water and brine
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-8b075205a83a475387d4f88b5acbb5ae
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785468B2

反応ノート

読み込み中…

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