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Triethylamine → Ethyl 3-(4-(5-fluoro-2,2-dimethyl-2,3-dihydrobenzofuran-7-carboxamido)phenyl)-2-methylpropanoate

HRID 2069695
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HRID 2069695 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:13]([OH:15])=O)[C:5]2[O:9][C:8]([CH3:11])([CH3:10])[CH2:7][C:6]=2[CH:12]=1.FC1C(F)=C(C(O)=O)C2OC(C)(C)CC=2C=1.[NH2:32][C:33]1[CH:38]=[CH:37][C:36]([CH2:39][CH:40]([CH3:46])[C:41]([O:43][CH2:44][CH3:45])=[O:42])=[CH:35][CH:34]=1.C(N(CC)CC)C.CCCP1(OP(CCC)(=O)OP(CCC)(=O)O1)=O>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([C:13]([NH:32][C:33]2[CH:34]=[CH:35][C:36]([CH2:39][CH:40]([CH3:46])[C:41]([O:43][CH2:44][CH3:45])=[O:42])=[CH:37][CH:38]=2)=[O:15])[C:5]2[O:9][C:8]([CH3:10])([CH3:11])[CH2:7][C:6]=2[CH:12]=1
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반응물 5

HCID 8471TriethylamineHCID 111923Propylphosphonic anhydrideHCID 46941402Ethyl 3-(4-aminophenyl)-2-methylpropanoateHCID 585663065,6-difluoro-2,2-dimethyl-3H-benzofuran-7-carboxylic acidHCID 585664155-Fluoro-2,2-dimethyl-2,3-dihydrobenzofuran-7-carboxylic acid

생성물 1

HCID 67405616
Ethyl 3-(4-(5-fluoro-2,2-dimethyl-2,3-dihydrobenzofuran-7-carboxamido)phenyl)-2-methylpropanoate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

5-fluoro-2,2-dimethyl-2,3-dihydrobenzofuran-7-carboxylic acid (803) (Compound was prepared in a similar manner as that described for the synthesis of (735) (101.3 mg, 0.482 mmol) was dissolved in dichloromethane (4 mL) and ethyl 3-(4-aminophenyl)-2-methylpropanoate (646) (100 mg, 0.482 mmol), triethyl amine (0.4 mL, 2.89 mmol), and 1-propanephosphonic acid cyclic anhydride (0.34 mL, 0.58 mmol, 50% in ethyl acetate) were added and stirred overnight at room temperature. The reaction was purified in vacuo and purified by flash column chromatography on silica gel with hexanes and EtOAc to give ethyl 3-(4-(5-fluoro-2,2-dimethyl-2,3-dihydrobenzofuran-7-carboxamido)phenyl)-2-methylpropanoate. The ester was dissolved in tetrahydrofuran (1.0 mL), methanol (1.0 mL) and water (3 mL). Lithium hydroxide was added and the reaction was stirred at room temperature for 4 h. The mixture was acidified with 1M HCl and diluted with EtOAc (3 mL). The organic layer was washed with brine (3 mL), dried over sodium sulfate and filtered. The filtrate was concentrated in vacuo to yield 3-(4-(5-fluoro-2,2-dimethyl-2,3-dihydrobenzofuran-7-carboxamido)phenyl)-2-methylpropanoic acid (97). 1H NMR (400 MHz, CDCl3) δ 9.53 (br, 1H), 7.66 (dd, J=9.9, 2.6 Hz, 1H), 7.57 (d, J=8.4 Hz, 2H), 7.19 (d, J=8.4 Hz, 2H), 7.02 (dd, J=9.9, 2.6 Hz, 1H), 3.13-3.00 (m, 3H), 2.72 (m, 2H), 1.60 (s, 6H), 1.19 (d, J=8.0 Hz, 3H).

후처리

  1. customThe reaction was purified in vacuo
  2. custompurified by flash column chromatography on silica gel with hexanes and EtOAc

출처 및 근거

ORD 기록
ord-c92821cc57eb4bafa109c2e30bc3a7fe
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08299117B2

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