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Triethylamine → N-[2-(4-valerylamino-1-piperidinyl)ethyl]-1-(2-propyl)-1H-indazole-3-carboxamide

HRID 2256369
ノート
印刷プレビュー

反応式

HRID 2256369 の反応式
C(O)(=O)C(O)=O.C(O)(=O)C(O)=O.[NH2:13][CH:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][NH:22][C:23]([C:25]2[C:33]3[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=3)[N:27]([CH:34]([CH3:36])[CH3:35])[N:26]=2)=[O:24])[CH2:16][CH2:15]1.C(N(CC)CC)C.[C:44](Cl)(=[O:49])[CH2:45][CH2:46][CH2:47][CH3:48]>O1CCCC1>[C:44]([NH:13][CH:14]1[CH2:15][CH2:16][N:17]([CH2:20][CH2:21][NH:22][C:23]([C:25]2[C:33]3[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=3)[N:27]([CH:34]([CH3:36])[CH3:35])[N:26]=2)=[O:24])[CH2:18][CH2:19]1)(=[O:49])[CH2:45][CH2:46][CH2:47][CH3:48]
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 61186Valeryl chlorideHCID 86751129N-[2-(4-amino-1-piperidinyl)ethyl]-1-(2-propyl)-1H-indazole-3-carboxamide dioxalate

生成物 1

HCID 10835560N-[2-(4-valerylamino-1-piperidinyl)ethyl]-1-(2-propyl)-1H-indazole-3-carboxamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The product from Example 23, as the free base (0.330 g, 1 mmol) and triethylamine (0.15 mL, 1.05 mmol) were stirred in 10.0 mL tetrahydrofuran and cooled briefly in an ice bath. To the mixture was added dropwise valeryl chloride (0.12 mL, 1 mmol) and the resulting mixture was stirred 18 h at room temperature and filtered, and the filtrate was evaporated to 0.385 g oil. Crystallization from diethyl ether provided 0.176 g colorless crystals. Mp 107°-109° C. Mass spectrum, m+ =413. Anal (C23H35N5O2) theory C, 66.80; H, 8.53; N, 16.93; found C, 66.59; H, 8.66; N, 17.04.

後処理

  1. temperaturecooled briefly in an ice bath
  2. filtrationfiltered
  3. customthe filtrate was evaporated to 0.385 g oil
  4. customCrystallization from diethyl ether

出典と根拠

ORDレコード
ord-6816039ac3a74ca89e3fa7006810eaeb
出典データセット
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05654320

反応ノート

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