Pyridine → HCID 67435761、化合物

HRID 1663390ノート

反応式

HRID 1663390 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:36]=[CH:37][CH:38]=1)[CH2:5][O:6][C:7]1[C:12]([Br:13])=[CH:11][C:10]([CH:14]2[C:23]3[C:22](=[O:24])[CH2:21][CH:20]([CH2:25][CH2:26][CH3:27])[CH2:19][C:18]=3[NH:17][C:16]([CH3:28])=[C:15]2[C:29]#[N:30])=[CH:9][C:8]=1[NH:31][S:32]([CH3:35])(=[O:34])=[O:33].N1C=CC=CC=1.[CH3:45][S:46](Cl)(=[O:48])=[O:47]>ClCCl.C(OCC)(=O)C>[Br:13][C:12]1[C:7]([O:6][CH2:5][C:4]2[CH:36]=[CH:37][CH:38]=[C:2]([NH:1][S:46]([CH3:45])(=[O:48])=[O:47])[CH:3]=2)=[C:8]([NH:31][S:32]([CH3:35])(=[O:34])=[O:33])[CH:9]=[C:10]([CH:14]2[C:23]3[C:22](=[O:24])[CH2:21][CH:20]([CH2:25][CH2:26][CH3:27])[CH2:19][C:18]=3[NH:17][C:16]([CH3:28])=[C:15]2[C:29]#[N:30])[CH:11]=1

参加物

6

反応物 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 67434762HCID 67434762、化合物

生成物 1

HCID 67435761HCID 67435761、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of N-[2-(3-amino-benzyloxy)-3-bromo-5-(3-cyano-2-methyl-5-oxo-7-propyl-1,4,5,6,7,8-hexahydro-quinolin-4-yl)-phenyl]-methanesulfonamide (709 mg) and pyridine (286 μl) in dichloromethane (20 ml) was added methanesulfonyl chloride (138 μl). After stirring for 18 h, the mixture was diluted with ethyl acetate and washed with water. The organic layer was dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by preparative HPLC (Method B).

後処理

  1. washwashed with water
  2. dry with materialThe organic layer was dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by preparative HPLC (Method B)

出典と根拠

ORDレコード
ord-975351b3708a465f85865e1f52495118
出典データセット
uspto-grants-2011_10
特許番号
US08034945B2

反応ノート

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