Pyridine → N-{3-Chloro-4-[4-(2-oxo-2H-3,1-benzoxazin-1(4H)-yl)piperidin-1-yl]phenyl}propane-2-sulfonamide

HRID 2414325

反応式

HRID 2414325 の反応式
[CH:1]([S:4](Cl)(=[O:6])=[O:5])([CH3:3])[CH3:2].[NH2:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]2[CH2:20][CH2:19][CH:18]([N:21]3[C:26]4[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=4[CH2:24][O:23][C:22]3=[O:31])[CH2:17][CH2:16]2)=[C:11]([Cl:32])[CH:10]=1.N1C=CC=CC=1>C(#N)C>[Cl:32][C:11]1[CH:10]=[C:9]([NH:8][S:4]([CH:1]([CH3:3])[CH3:2])(=[O:6])=[O:5])[CH:14]=[CH:13][C:12]=1[N:15]1[CH2:20][CH2:19][CH:18]([N:21]2[C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=3[CH2:24][O:23][C:22]2=[O:31])[CH2:17][CH2:16]1

参加物

5

反応物 3

HCID 1049PyridineHCID 824082-Propanesulfonyl chlorideHCID 226446801-[1-(4-Amino-2-chlorophenyl)piperidin-4-yl]-1,4-dihydro-2H-3,1-benzoxazin-2-one

生成物 1

HCID 22644580N-{3-Chloro-4-[4-(2-oxo-2H-3,1-benzoxazin-1(4H)-yl)piperidin-1-yl]phenyl}propane-2-sulfonamide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Isopropylsulphonyl chloride (0.03 ml) was added to a stirred solution of the product from example 120 step (ii) (0.05 g), pyridine (0.1 ml) in acetonitrile (0.9 ml) at room temperature. The mixture was stirred overnight, partitioned between ethyl acetate and water, the organics separated, washed with water, dried, and evaporated under reduced pressure. Purification was by chromatography eluting with 40% ethyl acetate/isohexane. Yield 0.015 g.

後処理

  1. custompartitioned between ethyl acetate and water
  2. washthe organics separated, washed with water
  3. customdried
  4. customevaporated under reduced pressure
  5. customPurification
  6. washeluting with 40% ethyl acetate/isohexane

出典と根拠

ORDレコード
ord-558892f7f8eb43d7a45a1efaf662520b
出典データセット
uspto-grants-2004_11
特許番号
US06812226B2

関連ノート

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