Pyridine → Trifluoromethanesulfonic acid 2-[4-((R)-3-dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-1-oxo-1,2,3,4-tetrahydroisoquinolin-6-yl ester

HRID 69414ノート

反応式

HRID 69414 の反応式
FC(F)(F)S([O:6][S:7]([C:10]([F:13])([F:12])[F:11])(=[O:9])=[O:8])(=O)=O.[CH3:16][N:17]([CH3:42])[C@@H:18]1[CH2:22][CH2:21][N:20]([C:23]2[CH:28]=[CH:27][C:26]([N:29]3[CH2:38][CH2:37][C:36]4[C:31](=[CH:32][CH:33]=[C:34](O)[CH:35]=4)[C:30]3=[O:40])=[CH:25][C:24]=2[F:41])[CH2:19]1.N1C=CC=CC=1>ClCCl>[CH3:16][N:17]([CH3:42])[C@@H:18]1[CH2:22][CH2:21][N:20]([C:23]2[CH:28]=[CH:27][C:26]([N:29]3[CH2:38][CH2:37][C:36]4[C:31](=[CH:32][CH:33]=[C:34]([O:6][S:7]([C:10]([F:11])([F:12])[F:13])(=[O:8])=[O:9])[CH:35]=4)[C:30]3=[O:40])=[CH:25][C:24]=2[F:41])[CH2:19]1

参加物

5

反応物 3

HCID 1049PyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 689879832-[4-((R)-3-Dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-6-hydroxy-3,4-dihydro-2H-isoquinolin-1-one

生成物 1

HCID 86635103Trifluoromethanesulfonic acid 2-[4-((R)-3-dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-1-oxo-1,2,3,4-tetrahydroisoquinolin-6-yl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoromethanesulfonic anhydride (2.06 g) was added to a solution of 2-[4-((R)-3-dimethylaminopyrrolidin-1-yl)-3-fluorophenyl]-6-hydroxy-3,4-dihydro-2H-isoquinolin-1-one (1.5 g) and pyridine (0.64 g) in dichloromethane (40 mL) at 0° C. After 30 minutes, the mixture was partitioned between water and dichloromethane, and the organic phase was dried over magnesium sulfate and concentrated. The product with the molecular weight of 501.50 (C22H23F4N3O4S) was obtained in this way; MS (ESI): 502 (M+H+).

後処理

  1. customthe mixture was partitioned between water and dichloromethane
  2. dry with materialthe organic phase was dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe product with the molecular weight of 501.50 (C22H23F4N3O4S) was obtained in this way

出典と根拠

ORDレコード
ord-8fd779e262d64cf6a87395e16586258a
出典データセット
uspto-grants-2014_09
特許番号
US08822495B2

反応ノート

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