Hydrochloric Acid → 1-(trans-4-Glycylamino-L-prolyl)-4-(3,5-dichlorophenoxy)piperidine Dihydrochloride

HRID 2185482ノート

反応式

HRID 2185482 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]([Cl:41])[CH:38]=[C:37]([Cl:42])[CH:36]=3)[CH2:30][CH2:29]2)=[O:27])[CH2:15]1)=[O:12])=O)(C)(C)C>O1CCOCC1>[ClH:41].[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:36]=[C:37]([Cl:42])[CH:38]=[C:39]([Cl:41])[CH:40]=3)[CH2:30][CH2:29]2)=[O:27])[CH2:15]1)=[O:12]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 701730401-[trans-4-(n-Tert-butoxycarbonylglycylamino)-n-tert-butoxycarbonyl-l-prolyl]-4-(3,5-dichlorophenoxy)piperidine

生成物 1

HCID 701757581-(trans-4-Glycylamino-L-prolyl)-4-(3,5-dichlorophenoxy)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 (13 mL) was added to a solution of 1-[trans-4-(N-tert-butoxycarbonylglycylamino)-N-tert-butoxycarbonyl-L-prolyl]-4-(3,5-dichlorophenoxy)piperidine (C, 640 mg) in 1,4-dioxane (13 mL) at room temperature. After stirring at room temperature for 30 min, the reaction mixture was evaporated in vacuo. The residue was washed with ether to give the titled compound (361 mg) as white crystals: 1H NMR (400 MHz, D2O) δ 1.80 (br s, 2H), 2.03 (br s, 2H), 2.40 (m, 1H), 2.61 (m, 1H), 3.46-3.50 (m, 2H), 3.60 (br s, 1H), 3.77 (m, 3H), 3.86 (s, 2H), 4.58 (br s, 1H), 4.72 (br s, 1H), 5.03 (t, J=8.3 Hz, 1H), 7.03 (br s, 2H), and 7.10 (br s, 1H); mass spectrum (EI+) m/e 415.

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-53b79b06cd154c7d823bf7859295fbc3
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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