Hydrochloric Acid → HCID 178484751, 화합물

HRID 2042728

반응식

HRID 2042728 반응식
[CH3:1][N:2]([C:8](=[O:31])[CH2:9][C@H:10]1[CH2:15][CH2:14][C@H:13]([C:16]2[CH:21]=[CH:20][C:19]([C:22]3[NH:26][N:25]=[C:24]([C:27]([F:30])([F:29])[F:28])[CH:23]=3)=[CH:18][CH:17]=2)[CH2:12][CH2:11]1)[CH2:3][C:4]([O:6]C)=[O:5].O1CCCC1.[OH-].[Li+].Cl>O>[CH3:1][N:2]([C:8](=[O:31])[CH2:9][C@H:10]1[CH2:11][CH2:12][C@H:13]([C:16]2[CH:17]=[CH:18][C:19]([C:22]3[CH:23]=[C:24]([C:27]([F:29])([F:30])[F:28])[NH:25][N:26]=3)=[CH:20][CH:21]=2)[CH2:14][CH2:15]1)[CH2:3][C:4]([OH:6])=[O:5]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 178501616HCID 178501616, 화합물

생성물 1

HCID 178484751HCID 178484751, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A 20 mL scintillation vial was charged with the product from Example 26D (12 mg, 0.027 mmol), 80% tetrahydrofuran in water, and lithium hydroxide (2.00 mg, 0.048 mmol) and shaken for 6 hours. After this time the reaction mixture was acidified with 1N HCl, filtered, and evaporated to dryness to afford the title product. The NMR spectrum includes a mixture of rotamers, with the major rotamer being reported. 1H NMR (500 MHz, DMSO-d6) δ ppm 1.02-1.20 (m, 2 H), 1.41-1.55 (m, 2 H), 1.74-1.91 (m, 5 H), 2.22-2.31 (m, 2 H), 2.78-2.80 (m, 1 H), 2.96-3.10 (m, 3 H), 3.98 (s, 2 H), 7.05-7.19 (m, 1 H), 7.27-7.45 (m, 2 H), 7.60-7.85 (m, 2 H), 13.98 (s, 1H): MS (ESI) m/z 424 [M+H]+.

후처리

  1. filtrationfiltered
  2. customevaporated to dryness

출처 및 근거

ORD 기록
ord-8a78aa0edb8e497abc7c9efcc3c7ed4b
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08586594B2

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