Dichloromethane → HCID 66899584、化合物

HRID 19419

反応式

HRID 19419 の反応式
C(OC(=O)[NH:7][C@H:8]([C:13](=[O:25])[NH:14][C:15]1[CH:19]=[CH:18][N:17]([CH2:20][C:21]([OH:24])([CH3:23])[CH3:22])[N:16]=1)[CH2:9][CH:10]([CH3:12])[CH3:11])(C)(C)C.FC(F)(F)C(O)=O.[Cl:34]CCl>>[ClH:34].[OH:24][C:21]([CH3:23])([CH3:22])[CH2:20][N:17]1[CH:18]=[CH:19][C:15]([NH:14][C:13](=[O:25])[C@@H:8]([NH2:7])[CH2:9][CH:10]([CH3:11])[CH3:12])=[N:16]1

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 67504285{(S)-1-[1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-ylcarbamoyl]-3-methyl-butyl}-carbamic acid t-butyl ester

生成物 1

HCID 66899584HCID 66899584、化合物収率 100%

実験手順

A solution of {(S)-1-[1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-ylcarbamoyl]-3-methyl-butyl}-carbamic acid t-butyl ester (4.15 g) in dichloromethane (8 mL) was treated with trifluoroacetic acid (8 mL) and stirred at room temperature for 1 h. At this time the mixture was concentrated in vacuo and the residue dissolved in methanol (10 mL) and treated with hydrogen chloride gas for 2 min. The mixture was concentrated in vacuo and the residue was dried under high vacuum. The solid obtained was triturated with diethyl ether which afforded (S)-2-amino-4-methyl-pentanoic acid [1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-yl]amide hydrochloride (3.86 g, 100%) as a white solid.

後処理

  1. concentrationAt this time the mixture was concentrated in vacuo
  2. dissolutionthe residue dissolved in methanol (10 mL)
  3. additiontreated with hydrogen chloride gas for 2 min
  4. concentrationThe mixture was concentrated in vacuo
  5. customthe residue was dried under high vacuum
  6. customThe solid obtained
  7. customwas triturated with diethyl ether which

出典と根拠

ORDレコード
ord-152031cee96541c2bd021b434ddece9f
出典データセット
uspto-grants-2010_06
特許番号
US07741327B2

関連ノート

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