Hydrochloric Acid → HCID 67334527、化合物

HRID 1670631ノート

反応式

HRID 1670631 の反応式
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][C@@H:12]([NH:15][C:16]2[CH:21]=[CH:20][C:19]([Br:22])=[CH:18][C:17]=2[N+:23]([O-:25])=[O:24])[C@H:11]([OH:26])[CH2:10]1)=O)(C)(C)C>O1CCOCC1.ClCCl>[ClH:1].[Br:22][C:19]1[CH:20]=[CH:21][C:16]([NH:15][C@@H:12]2[CH2:13][CH2:14][NH:9][CH2:10][C@H:11]2[OH:26])=[C:17]([N+:23]([O-:25])=[O:24])[CH:18]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 67335873(3R,4R)-4-(4-Bromo-2-nitro-phenylamino)-3-hydroxy-piperidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 67334527HCID 67334527、化合物収率 89%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

実験手順

Add 4.0 M hydrogen chloride in dioxane (70 mL) slowly to a solution of (3R,4R)-4-(4-bromo-2-nitro-phenylamino)-3-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (0.027 mol, 11.5 g) in dry dichloromethane (40 mL) at room temperature and stir for 16 h. Filter the precipitate and dry under vacuum to obtain the title compound (8.68 g, 89%) as a yellow solid. 1H NMR (400 MHz, CD3OD) δ 1.81-1.86 (m, 1H), 2.39-2.44 (m, 1H), 3.02-3.07 (m, 1H), 3.18-3.26 (m, 1H), 3.34-3.40 (m, 1H), 3.45 (dd, 1H), 3.87-3.91 (m, 2H), 7.17 (d, 1H), 7.61 (dd, 1H), 8.28 (d, 1H).

後処理

  1. filtrationFilter the precipitate
  2. customdry under vacuum

出典と根拠

ORDレコード
ord-eba2ef889b814b6ba150b250fe7fceb5
出典データセット
uspto-grants-2011_08
特許番号
US07994164B2

反応ノート

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