Trifluoroacetic acid → HCID 66628192、化合物

HRID 2200989ノート

反応式

HRID 2200989 の反応式
[C:1]([C:3]1[C@@H:8]([C:9]2[CH:14]=[CH:13][C:12]([C:15]#[N:16])=[CH:11][CH:10]=2)[N:7]2[N:17]=[C:18]([NH:20][CH2:21][C:22]([O:24]C(C)(C)C)=[O:23])[N:19]=[C:6]2[N:5]([C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([C:35]([F:38])([F:37])[F:36])[CH:30]=2)[C:4]=1[CH3:39])#[N:2].FC(F)(F)C(O)=O>ClCCl>[C:1]([C:3]1[C@@H:8]([C:9]2[CH:14]=[CH:13][C:12]([C:15]#[N:16])=[CH:11][CH:10]=2)[N:7]2[N:17]=[C:18]([NH:20][CH2:21][C:22]([OH:24])=[O:23])[N:19]=[C:6]2[N:5]([C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([C:35]([F:37])([F:38])[F:36])[CH:30]=2)[C:4]=1[CH3:39])#[N:2]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acid2 回HCID 46841208HCID 46841208、化合物

生成物 1

HCID 66628192HCID 66628192、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Under an atmosphere of argon protective gas, tert-butyl N-{(7R)-6-cyano-7-(4-cyanophenyl)-5-methyl-4-[3-(trifluoromethyl)phenyl]-4,7-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-2-yl}glycinate (18.0 mg, 34 μmol) was dissolved in dry dichloromethane (3.1 ml). At room temperature, trifluoroacetic acid (1.6 ml) was added, and the mixture was stirred for 45 min. More trifluoroacetic acid (2 ml) was then added, and the mixture was stirred for a further 30 min. The reaction mixture was then concentrated under reduced pressure and the residue was purified by preparative HPLC (Gromsil C18 column, 30×250 mm; mobile phase: acetonitrile-water-0.1% TFA). After lyophilization, the product was obtained as a solid (15.2 mg, 94% of theory).

後処理

  1. stirringthe mixture was stirred for a further 30 min
  2. concentrationThe reaction mixture was then concentrated under reduced pressure
  3. customthe residue was purified by preparative HPLC (Gromsil C18 column, 30×250 mm; mobile phase: acetonitrile-water-0.1% TFA)
  4. customAfter lyophilization, the product was obtained as a solid (15.2 mg, 94% of theory)

出典と根拠

ORDレコード
ord-354aa7a0acf64c66a35de3acd88b369d
出典データセット
uspto-grants-2016_06
特許番号
US09359362B2

反応ノート

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