Formaldehyde → Ro4368554

HRID 1005662노트

반응식

HRID 1005662 반응식
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

참가 물질

5

반응물 2

HCID 712FormaldehydeHCID 69351600HCID 69351600, 화합물

생성물 1

HCID 6918682Ro4368554

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3a751f096c5a485a935238028a02882b
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787535B2

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