Triethylamine → HCID 73292226, 화합물

HRID 1398036노트

반응식

HRID 1398036 반응식
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

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 86722002HCID 86722002, 화합물HCID 86722003HCID 86722003, 화합물

생성물 1

HCID 73292226HCID 73292226, 화합물수율 52.5%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fd87fad3e1eb4df691254c69f8ee3219
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08901314B2

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