Hydrochloric Acid → 1-(trans-4-Glycylamino-L-Prolyl)-4-(2-Chloro-5-Methylphenoxy)piperidine Dihydrochloride

HRID 2185487ノート

反応式

HRID 2185487 の反応式
[ClH:1].C(OC([NH:9][CH2:10][C:11]([NH:13][C@H:14]1[CH2:18][N:17](C(OC(C)(C)C)=O)[C@H:16]([C:26]([N:28]2[CH2:33][CH2:32][CH:31]([O:34][C:35]3[CH:40]=[C:39]([CH3:41])[CH:38]=[CH:37][C:36]=3[Cl:42])[CH2:30][CH2:29]2)=[O:27])[CH2:15]1)=[O:12])=O)(C)(C)C>O1CCOCC1>[ClH:42].[ClH:1].[NH2:9][CH2:10][C:11]([NH:13][C@H:14]1[CH2:18][NH:17][C@H:16]([C:26]([N:28]2[CH2:33][CH2:32][CH:31]([O:34][C:35]3[CH:40]=[C:39]([CH3:41])[CH:38]=[CH:37][C:36]=3[Cl:42])[CH2:30][CH2:29]2)=[O:27])[CH2:15]1)=[O:12]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 701767841-[trans-4-(n-Tert-butoxycarbonylglycylamino)-n-tert-butoxycarbonyl-l-prolyl]-4-(2-chloro-5-methylphenoxy)piperidine

生成物 1

HCID 701771821-(trans-4-Glycylamino-L-Prolyl)-4-(2-Chloro-5-Methylphenoxy)piperidine Dihydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

A solution of 4 N hydrochloric acid in 1,4-dioxane (8 mL) was added to a solution of 1-[trans-4-(N-tert-butoxycarbonylglycylamino)-N-tert-butoxycarbonyl-L-prolyl]-4-(2-chloro-5-methylphenoxy)piperidine (C, 280 mg) in 1,4-dioxane (8 mL) at room temperature. After stirring at room temperature for 20 min, the reaction mixture was evaporated in vacuo. The residue was washed with ether to give the titled compound (142 mg) as a white powder: 1H NMR (400 MHz, D2O) δ 1.90-2.01 (4H), 2.32 (s, 3H), 2.43 (m, 1H), 2.61 (br s, 1H), 3.49 (br t, 2H), 3.67 (br s, 1H), 3.79 (m, 4H), 3.85 (s, 2H), 4.58 (br s, 1H), 5.02 (m, 1H), 6.91 (d, J=8.0 Hz, 1H), 7.09 (s, 1H), and 7.35 (d, J=8.0 Hz, 1H); mass spectrum (EI+) m/e 394 (M).

後処理

  1. customthe reaction mixture was evaporated in vacuo
  2. washThe residue was washed with ether

出典と根拠

ORDレコード
ord-6a6ae7232a1e4d7bbe5234bc4abf8c76
出典データセット
uspto-grants-2002_06
特許番号
US06399629B1

反応ノート

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