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Triethylamine → HCID 57639703、化合物

HRID 909207
ノート
印刷プレビュー

反応式

HRID 909207 の反応式
O=C1CCC(=O)N1O[C:9]([C:11]1[CH:19]=[C:18]2[C:14]([CH:15]=[N:16][N:17]2[CH2:20][CH:21]([CH3:23])[CH3:22])=[CH:13][C:12]=1[O:24][C:25]1[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:26]=1[F:32])=[O:10].Cl.Cl.[CH3:35][O:36][C:37](=[O:45])[CH:38]([NH2:44])[CH2:39][CH2:40][N:41]([CH3:43])[CH3:42].C(N(CC)CC)C>ClCCl>[CH3:35][O:36][C:37](=[O:45])[C@@H:38]([NH:44][C:9]([C:11]1[CH:19]=[C:18]2[C:14]([CH:15]=[N:16][N:17]2[CH2:20][CH:21]([CH3:23])[CH3:22])=[CH:13][C:12]=1[O:24][C:25]1[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:26]=1[F:32])=[O:10])[CH2:39][CH2:40][N:41]([CH3:43])[CH3:42]
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 8471TriethylamineHCID 426324812,5-dioxopyrrolidin-1-yl 5-(2,4-difluorophenoxy)-1-isobutyl-1H-indazole-6-carboxylateHCID 57418767HCID 57418767、化合物

生成物 1

HCID 57639703HCID 57639703、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-(2,4-difluorophenoxy)-1-isobutyl-1H-indazole-6-carboxylic acid 2,5-dioxopyrrolidin-1-yl ester (32.0 g, 72.2 mmol) and 2-amino-4-dimethylaminobutyric acid methyl ester dihydrochloride (19.35 g, 83.0 mmol) in dichloromethane was added triethylamine (35 mL, 253 mmol) and the mixture stirred at room temperature for 4 hours. The reaction mixture was concentrated under reduced pressure and diluted with dichloromethane (400 mL). The solution was washed with saturated NH4Cl (2×200 mL), saturated NaHCO3 (2×200 mL) and brine (200 mL). The organics were dried over MgSO4 and concentrated under reduced pressure to afford the crude product.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additiondiluted with dichloromethane (400 mL)
  3. washThe solution was washed with saturated NH4Cl (2×200 mL), saturated NaHCO3 (2×200 mL) and brine (200 mL)
  4. dry with materialThe organics were dried over MgSO4
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-87b06249c6b64a3382830c0e7f204cb7
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08017641B2

反応ノート

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