Ammonium Hydroxide → 1-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carboxamide

HRID 549238ノート

反応式

HRID 549238 の反応式
Cl.C[N:3](C)CCCN=C=NCC.[CH2:13]([N:16]1[C:20]([CH2:21][CH:22]2[CH2:27][CH2:26][O:25][CH2:24][CH2:23]2)=[CH:19][C:18]([C:28]([OH:30])=O)=[N:17]1)[CH2:14][CH3:15].ON1C2C=CC=CC=2N=N1.[OH-].[NH4+]>CN(C)C=O.O>[CH2:13]([N:16]1[C:20]([CH2:21][CH:22]2[CH2:27][CH2:26][O:25][CH2:24][CH2:23]2)=[CH:19][C:18]([C:28]([NH2:3])=[O:30])=[N:17]1)[CH2:14][CH3:15]

参加物

7

反応物 4

HCID 14923Ammonium HydroxideHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 671577251-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carboxylic acid

生成物 1

HCID 671577891-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carboxamide収率 83.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (4.06 g, 21.2 mmol) was added to a solution of 1-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carboxylic acid (4.88 g, 19.3 mmol) and 1-hydroxybenzotriazole (2.87 g, 21.2 mmol) in N,N-dimethylformamide (DMF) (24.4 mL) at room temperature. The mixture was stirred for two hours, cooled in an ice bath, and treated with concentrated ammonium hydroxide (3.9 mL). A precipitate formed, and the mixture was stirred 30 minutes at 0° C. Water (100 mL) was added, and the mixture was stirred for an additional ten minutes. The precipitate was isolated by filtration, washed with water, and dried on the vacuum filter funnel to provide 4.05 g of 1-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carboxamide as white crystals.

後処理

  1. temperaturecooled in an ice bath
  2. customA precipitate formed
  3. stirringthe mixture was stirred 30 minutes at 0° C
  4. stirringthe mixture was stirred for an additional ten minutes
  5. customThe precipitate was isolated by filtration
  6. washwashed with water
  7. customdried on the vacuum
  8. filtrationfilter funnel

出典と根拠

ORDレコード
ord-6d08184d45bb454bab2f08f5333c89bf
出典データセット
uspto-grants-2011_05
特許番号
US07943636B2

反応ノート

読み込み中…