Isoquinoline-1-carboxylic acid → HCID 178481697、化合物

HRID 33221

反応式

HRID 33221 の反応式
OC1C2N=NNC=2C=CC=1.Cl.CN(C)CCCN=C=NCC.[CH3:23][NH:24][C:25](=[S:28])[NH:26][NH2:27].[C:29]1([C:39](O)=O)[C:38]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[CH:32]=[CH:31][N:30]=1>CN(C)C=O.C(N(CC)CC)C>[C:29]1([C:39]2[N:24]([CH3:23])[C:25]([SH:28])=[N:26][N:27]=2)[C:38]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[CH:32]=[CH:31][N:30]=1

参加物

7

実験手順

Hydroxybenzotriazole (0.078 g), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.11 g) and triethylamine were added successively to a cooled solution (0° C.) of 4-methyl-3-thiosemicarbazide (0.061 g) and 1-isoquinoline carboxylic acid (0.10 g) in dimethylformamide (3 ml). Following addition the cooling bath was removed and the mixture was stirred at room temperature over night and then the reaction mixture was evaporated to dryness. To the residue was added sodium hydroxide solution (0.5 M, 5 ml) and the mixture was stirred at 80° C. for 3 h. The mixture was cooled to room temperature and the pH adjusted to pH 6 using hydrochloric acid solution (2M) and the resulting precipitate was filtered and dried in vacuo to give the title compound (0.11 g, 78%) as an off-white solid.

後処理

  1. additionaddition the cooling bath
  2. customwas removed
  3. customthe reaction mixture was evaporated to dryness
  4. additionTo the residue was added sodium hydroxide solution (0.5 M, 5 ml)
  5. stirringthe mixture was stirred at 80° C. for 3 h
  6. temperatureThe mixture was cooled to room temperature
  7. filtrationthe resulting precipitate was filtered
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-bf1242f4a62f4ab2a9d086f066f1c384
出典データセット
uspto-grants-2008_09
特許番号
US07429579B2

関連ノート

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