Hydrochloric Acid → Ethyl (1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-acetate hydrochloride

HRID 2236093ノート

反応式

HRID 2236093 の反応式
C(OC([N:8]1[CH2:26][CH2:25][C:11]2[N:12]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=3[C:10]=2[CH2:9]1)=O)(C)(C)C.[ClH:27]>C(OCC)(=O)C>[ClH:27].[CH2:9]1[C:10]2[C:18]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[N:12]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:11]=2[CH2:25][CH2:26][NH:8]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 71063767Ethyl (2-tert-butoxycarbonyl-1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-acetate

生成物 1

HCID 71552668Ethyl (1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-acetate hydrochloride収率 79%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

A solution of ethyl (2-tert.-butoxycarbonyl-1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-acetate (8.45 g, 23.6 mmol) in ethyl acetate (80 ml) is treated with a solution of 3M HCl in ethyl acetate (39.3 ml). After stirring at room temperature for 3 h, the solvent is removed in vacuo and the residue azeotroped twice with toluene. The crude product is suspended in diethyl ether, filtered off, washed with diethyl ether and dried. Finally, pure title compound is obtained as beige solid (5.49 g) in 79% yield. tR (LC-2) 1.41 min; ESL-MS (positive ion): m/z 259.33 [M+H]+ (calcd 258.32 for C15H18N2O2).

後処理

  1. customthe solvent is removed in vacuo
  2. customthe residue azeotroped twice with toluene
  3. filtrationfiltered off
  4. washwashed with diethyl ether
  5. customdried

出典と根拠

ORDレコード
ord-f773c64b2dfe498e933999e41fe0dbf4
出典データセット
uspto-grants-2010_05
特許番号
US07714132B2

反応ノート

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