Hydrochloric Acid → HCID 67334527, 화합물

HRID 1670631노트

반응식

HRID 1670631 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 67334527HCID 67334527, 화합물수율 89%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  1. filtrationFilter the precipitate
  2. customdry under vacuum

출처 및 근거

ORD 기록
ord-eba2ef889b814b6ba150b250fe7fceb5
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994164B2

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