Formaldehyde → Ro4368554

HRID 1005662ノート

反応式

HRID 1005662 の反応式
Cl.[C:2]1([S:8]([C:11]2[C:19]3[C:14](=[C:15]([N:20]4[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]4)[CH:16]=[CH:17][CH:18]=3)[NH:13][CH:12]=2)(=[O:10])=[O:9])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:26]=O>C(O)C.[Pd]>[C:2]1([S:8]([C:11]2[C:19]3[C:14](=[C:15]([N:20]4[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]4)[CH:16]=[CH:17][CH:18]=3)[NH:13][CH:12]=2)(=[O:9])=[O:10])[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 712FormaldehydeHCID 69351600HCID 69351600、化合物

生成物 1

HCID 6918682Ro4368554

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A solution of 3-benzenesulfonyl-7-piperazin-1-yl-1H-indole (101) (500 mg, 1.46 mmol) and 1 mL of 37% aqueous formaldehyde in 25 mL of ethanol was hydrogenated at atmospheric pressure in the presence of 250 mg of 10% Pd-C for 30 min. The mixture was filtered, diluted with water and extracted with ethyl acetate. The ethyl acetate was washed with water and brine, dried, and evaporated to yield the crude free base of 3-benzenesulfonyl-7-(4-methyl-piperazin-1-yl)-1H-indole. The hydrochloride salt was crystallized from ethanol-ether to afford 290 mg of (501), m.p. 160-162° C.

後処理

  1. filtrationThe mixture was filtered
  2. additiondiluted with water
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate was washed with water and brine
  5. customdried
  6. customevaporated

出典と根拠

ORDレコード
ord-3a751f096c5a485a935238028a02882b
出典データセット
uspto-grants-2004_09
特許番号
US06787535B2

反応ノート

読み込み中…