Hydrochloric Acid → HCID 59336110、化合物

HRID 2046360ノート

反応式

HRID 2046360 の反応式
Cl.[CH:2]1([CH2:8][N:9]2[CH2:14][CH2:13][CH:12]([N:15]([CH3:36])[C:16](=[O:35])[CH2:17][O:18][C:19]3[N:24]=[C:23]([CH3:25])[C:22]([NH:26]C(=O)OC(C)(C)C)=[C:21]([CH3:34])[N:20]=3)[CH2:11][CH2:10]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.[OH-].[Na+]>C(Cl)(Cl)Cl>[NH2:26][C:22]1[C:23]([CH3:25])=[N:24][C:19]([O:18][CH2:17][C:16]([N:15]([CH:12]2[CH2:13][CH2:14][N:9]([CH2:8][CH:2]3[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]3)[CH2:10][CH2:11]2)[CH3:36])=[O:35])=[N:20][C:21]=1[CH3:34]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59336176Tert-butyl 2-(2-((1-(cyclohexylmethyl)piperidine-4-yl)(methyl)amino)-2-oxoethoxy)-4,6-dimethylpyrimidine-5-ylcarbamate

生成物 1

HCID 59336110HCID 59336110、化合物収率 76%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

6N HCl (0.7 mL) was added to a chloroform (0.5 mL) solution of Compound 32 (39 mg) and the mixture was stirred at room temperature for 1 hour. While the reaction mixture was cooled with ice, a 4N aqueous sodium hydroxide solution was added to neutralize the mixture. The resulting product was extracted with chloroform and the organic layer was dried over sodium sulfate, filtered, and concentrated under reduced pressure. The resulting residue was purified by amino-coated silica gel (Fuji Sylysia Chemical Ltd., NH-DM1020) column chromatography (ethyl acetate) to give 23 mg (76% yield) of the title compound.

後処理

  1. temperatureWhile the reaction mixture was cooled with ice
  2. extractionThe resulting product was extracted with chloroform
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by amino-coated silica gel (Fuji Sylysia Chemical Ltd., NH-DM1020) column chromatography (ethyl acetate)

出典と根拠

ORDレコード
ord-77650a83b32540639fab1e9c5c98be17
出典データセット
uspto-grants-2013_11
特許番号
US08592435B2

反応ノート

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