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

HRID 1063240ノート

反応式

HRID 1063240 の反応式
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

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-7f07e52592a74a57b67846dfc85103e9
出典データセット
uspto-grants-2005_11
特許番号
US06964970B2

反応ノート

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