Trifluoroacetic acid → HCID 178493513、化合物

HRID 1778787ノート

反応式

HRID 1778787 の反応式
[F:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[C:4]([F:12])[C:3]=1[C:13]1[N:18]=[C:17]2[NH:19][N:20]=[C:21]([C:22]3[CH:31]=[C:30]4[C:25]([CH2:26][CH2:27][N:28](C(OC(C)(C)C)=O)[CH2:29]4)=[CH:24][CH:23]=3)[C:16]2=[CH:15][N:14]=1.C(O)(C(F)(F)F)=O.[CH3:46][S:47](Cl)(=[O:49])=[O:48]>ClCCl.CO>[F:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([O:10][CH3:11])=[C:4]([F:12])[C:3]=1[C:13]1[N:18]=[C:17]2[NH:19][N:20]=[C:21]([C:22]3[CH:31]=[C:30]4[C:25]([CH2:26][CH2:27][N:28]([S:47]([CH3:46])(=[O:49])=[O:48])[CH2:29]4)=[CH:24][CH:23]=3)[C:16]2=[CH:15][N:14]=1

参加物

6

反応物 3

HCID 6422Trifluoroacetic acidHCID 31297Methanesulfonyl chlorideHCID 178493512tert-butyl 7-[6-(2,6-difluoro-3,5-dimethoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-3-yl]-3,4-dihydroisoquinoline-2(1H)-carboxylate

生成物 1

HCID 178493513HCID 178493513、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

tert-Butyl 7-[6-(2,6-difluoro-3,5-dimethoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-3-yl]-3,4-dihydroisoquinoline-2(1H)-carboxylate (10.0 mg, 0.0191 mmol) in dichloromethane (0.10 mL) was treated with TFA (0.10 mL). The mixture was stirred at r.t. for 1 h. The volatiles were evaporated. The residue was dissolved in acetonitrile (0.5 mL) and N,N-diisopropylethylamine (30.0 μL). To the mixture was added methanesulfonyl chloride (2.0 μL, 0.026 mmol). The mixture was stirred at r.t. for 30 min, and then diluted with methanol, and purified by RP-HPLC (pH=10) to afford the desired product. LCMS (M+H)+=502.1.

後処理

  1. customThe volatiles were evaporated
  2. dissolutionThe residue was dissolved in acetonitrile (0.5 mL)
  3. stirringThe mixture was stirred at r.t. for 30 min
  4. custompurified by RP-HPLC (pH=10)

出典と根拠

ORDレコード
ord-0d8ca70b511740faafef1e0e016157a0
出典データセット
uspto-grants-2016_02
特許番号
US09266892B2

反応ノート

読み込み中…