Triethylamine → HCID 73292226、化合物

HRID 1398036ノート

反応式

HRID 1398036 の反応式
Cl.[NH:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]([CH3:12])[CH3:11])[NH2:3].[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([C:20](=O)[CH2:21][C:22]([CH:24]2[CH2:29][C:28]([CH3:31])([CH3:30])[O:27][C:26]([CH3:33])([CH3:32])[CH2:25]2)=O)=[CH:16][CH:15]=1.C(N(CC)CC)C>CO.CCOC(C)=O>[Cl:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]2[N:2]([C:4]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[N:10]([CH3:12])[CH3:11])[N:3]=[C:22]([CH:24]3[CH2:25][C:26]([CH3:33])([CH3:32])[O:27][C:28]([CH3:31])([CH3:30])[CH2:29]3)[CH:21]=2)=[CH:18][CH:19]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 86722002HCID 86722002、化合物HCID 86722003HCID 86722003、化合物

生成物 1

HCID 73292226HCID 73292226、化合物収率 52.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of (2-hydrazino-phenyl)-dimethyl-amine hydrochloride (105 mg, 0.56 mmol), 1-(4-chloro-phenyl)-3-(2,2,6,6-tetramethyl-tetrahydro-pyran-4-yl)-propane-1,3-dione (162 mg, 0.50 mmol), and triethylamine (0.08 mL, 0.56 mmol), in 1.4 mL of methanol was stirred at RT for 8 hrs. The mixture was diluted with 20 mL of EtOAc and washed with saturated NaHCO3 (40 mL) and brine (40 mL). The organic layer was dried over Na2SO4, concentrated, and the residue purified by flash chromatography on silica gel to give 115 mg (47%) of the title compound as a white solid.

後処理

  1. washwashed with saturated NaHCO3 (40 mL) and brine (40 mL)
  2. dry with materialThe organic layer was dried over Na2SO4
  3. concentrationconcentrated
  4. customthe residue purified by flash chromatography on silica gel

出典と根拠

ORDレコード
ord-fd87fad3e1eb4df691254c69f8ee3219
出典データセット
uspto-grants-2014_12
特許番号
US08901314B2

反応ノート

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