Hydrochloric Acid → 2,2-Dimethyl-3-(2-(7-methyl-[1,2,4]triazolo[4,3-a]pyridin-3-yl)quinolin-8-yloxy)propan-1-amine trihydrochloride

HRID 876510ノート

反応式

HRID 876510 の反応式
[CH3:1][C:2]([CH3:34])([CH2:12][O:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[C:21]([C:24]1[N:28]3[CH:29]=[CH:30][C:31]([CH3:33])=[CH:32][C:27]3=[N:26][N:25]=1)[CH:20]=[CH:19]2)[CH2:3][NH:4]C(=O)OC(C)(C)C.[ClH:35]>ClCCl>[ClH:35].[ClH:35].[ClH:35].[CH3:1][C:2]([CH3:34])([CH2:12][O:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[C:21]([C:24]1[N:28]3[CH:29]=[CH:30][C:31]([CH3:33])=[CH:32][C:27]3=[N:26][N:25]=1)[CH:20]=[CH:19]2)[CH2:3][NH2:4]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67230779Tert-butyl 2,2-dimethyl-3-(2-(7-methyl-[1,2,4]triazolo[4,3-a]pyridin-3-yl)quinolin-8-yloxy)propylcarbamate

生成物 1

HCID 672331932,2-Dimethyl-3-(2-(7-methyl-[1,2,4]triazolo[4,3-a]pyridin-3-yl)quinolin-8-yloxy)propan-1-amine trihydrochloride収率 70%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of tert-butyl 2,2-dimethyl-3-(2-(7-methyl-[1,2,4]triazolo[4,3-a]pyridin-3-yl)quinolin-8-yloxy)propylcarbamate (35 mg, 0.076 mmol) and hydrochloric acid (4 M in dioxane, 0.57 mL, 2.3 mmol) in dichloromethane (0.5 mL) was stirred overnight. The reaction was concentrated under reduced pressure. The residue was evaporated from twice from toluene, once from hexanes, triturated with hexanes, filtered and dried in vacuo to provide 25 mg (70%) of desired product as the trihydrochloride salt. MS ESI (+) m/z 362 (M+1) detected.

後処理

  1. concentrationThe reaction was concentrated under reduced pressure
  2. customThe residue was evaporated from twice from toluene
  3. customonce from hexanes, triturated with hexanes
  4. filtrationfiltered
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-2900ba3aa5ae4292a26bf23af6c8eab8
出典データセット
uspto-grants-2015_03
特許番号
US08987251B2

反応ノート

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