Hydrochloric Acid → 9-methyl-1,3,4,9-tetrahydro-2H-pyrido[3,4-b]-indole mono hydrochloride

HRID 1063240노트

반응식

HRID 1063240 반응식
C(OC([N:11]1[CH2:23][CH2:22][C:21]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[N:14]([CH3:24])[C:13]=2[CH2:12]1)=O)C1C=CC=CC=1.[ClH:25]>CO.CCOC(C)=O.[Pd]>[ClH:25].[CH3:24][N:14]1[C:15]2[C:20](=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:21]2[CH2:22][CH2:23][NH:11][CH2:12][C:13]1=2

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 120692932-benzyloxycarbonyl-9-methyl-1,3,4,9-tetrahydro-2H-pyrido[3,4-b]indole

생성물 1

HCID 224011859-methyl-1,3,4,9-tetrahydro-2H-pyrido[3,4-b]-indole mono hydrochloride수율 92%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-benzyloxycarbonyl-9-methyl-1,3,4,9-tetrahydro-2H-pyrido[3,4-b]indole (5.17 g. 16.2 mmole) in methanol (100 mL), EtOAc (25 mL) and HCl (17 mL, 1M in dioxane) at RT in a Parr hydrogenation flask was added 10% Pd/C (0.5 g). The reaction mixture was shaken under 45 psi of H2 for 6 hr. The suspension was filtered through celite®), and the filter pad was washed with methanol. The filtrate was concentrated on the rotavap, and the residue was dried under high vacuum to afford the titled compound (3.19 g. 92%) as a white solid: MS (ES) m/e 187 (M+H−HCl)+.

후처리

  1. filtrationThe suspension was filtered through celite®), and the filter pad
  2. washwas washed with methanol
  3. concentrationThe filtrate was concentrated on the rotavap
  4. customthe residue was dried under high vacuum

출처 및 근거

ORD 기록
ord-7f07e52592a74a57b67846dfc85103e9
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06964970B2

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