Hydrochloric Acid → HCID 178492505、化合物

HRID 70056

反応式

HRID 70056 の反応式
[C:1]1([NH:7][C:8]2[N:9](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH:10]=[C:11]([C:13]([C:15]3[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[C:17]([O:25][CH3:26])[CH:16]=3)=[O:14])[N:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl>C(OCC)C>[C:1]1([NH:7][C:8]2[NH:9][CH:10]=[C:11]([C:13]([C:15]3[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[C:17]([O:25][CH3:26])[CH:16]=3)=[O:14])[N:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 66780583(2-(Phenylamino)-1-trityl-1H-imidazol-4-yl)(3,4,5 trimethoxyphenyl)methanone

生成物 1

HCID 178492505HCID 178492505、化合物収率 63%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a solution of trityl protected compound (e) (50 mg, 0.084 mmol) in ethyl ether was added 2 M HCl in ether (1 mL, 1 mmol). The reaction mixture was stirred overnight and washed with saturated NaHCO3 and dried with MgSO4. Filtration and evaporation of the solvent followed by flash chromatography to yield de-protection compound 5e (18 mg, 63%). 1H NMR (500 MHz, DMSO-d6) δ 7.54 (s, br, 1H), 7.51-7.43 (m, 3H), 7.33 (d, 2H), 7.04 (s, 2H), 6.62 (br, 2H) 3.82 (s, 6H), 3.73 (s, 3H). MS: 352.1 (M−H)−; 354.3 (M+H)+.

後処理

  1. washwashed with saturated NaHCO3
  2. dry with materialdried with MgSO4
  3. filtrationFiltration and evaporation of the solvent

出典と根拠

ORDレコード
ord-beaa4214eef14190913007d5d1c33b8a
出典データセット
uspto-grants-2014_09
特許番号
US08822513B2

関連ノート

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