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Water → HCID 44199535, 화합물

HRID 602290
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HRID 602290 반응식
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([CH2:10][N:11]2[CH2:16][CH2:15][O:14][CH:13]([C:17](OC(C)(C)C)=O)[CH:12]2CN)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].FC(F)(F)C(O)=O.[NH2:33][C:34]1[C:42]2[CH2:41][CH2:40][O:39][C:38]=2[C:37]([C:43](O)=[O:44])=[CH:36][C:35]=1[Cl:46].O.C[N:49](C=O)C>C(Cl)Cl>[C:1]([N:4]1[CH2:5][CH2:6][CH:7]([CH2:10][N:11]2[CH2:16][CH2:15][O:14][CH:13]([CH2:17][NH:49][C:43]([C:37]3[C:38]4[O:39][CH2:40][CH2:41][C:42]=4[C:34]([NH2:33])=[C:35]([Cl:46])[CH:36]=3)=[O:44])[CH2:12]2)[CH2:8][CH2:9]1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 962WaterHCID 6228DimethylformamideHCID 6422Trifluoroacetic acidHCID 106324014-Amino-5-chloro-2,3-dihydrobenzofuran-7-carboxylic acidHCID 1317287484-(1-Acetyl-4-piperidinylmethyl)-2-(tert-butoxycarbonyl)-aminomethylmorpholine

생성물 1

HCID 44199535HCID 44199535, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-(1-acetyl-4-piperidinylmethyl)-2-(tert -butoxycarbonyl)-aminomethylmorpholine (Reference Example 15) (0.70 g) in methylene chloride (5 ml) was added trifluoroacetic acid (5 ml), and the mixture was stirred at room temperature for 2 hours. The reaction solution was dried under reduced pressure to be solidified, and the residue was dissolved in toluene, and then dried under reduced pressure to be solidified again. To the residue was added water, and the mixture was alkalified with 2N aqueous sodium hydroxide and extracted with chloroform. The extract was washed with water, then brine, and then dried over anhydrous magnesium sulfate. The solvent was removed in vacuo. A solution of the oily residue in DMF (5 ml) containing 4-(1-acetyl-4-piperidinylmethyl)-2-aminomethylmorpholine was added to a reaction solution which was obtained by stirring a solution of 4-amino-5-chloro-2, 3-dihydrobenzo[b]furan-7-carboxylic acid (0.42 g) and N,N′-carbonyldiimidazole (0.35 g) in DMF (10 ml) at room temperature for 1 hour. The mixture was stirred at room temperature overnight. To the reaction solution was added water, and the mixture was extracted with chloroform, and then the extract was sequentially washed with saturated sodium bicarbonate, water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol=30/1) to give the titled compound (0.85 g) as a white amorphous solid.

후처리

  1. customThe reaction solution was dried under reduced pressure
  2. dissolutionthe residue was dissolved in toluene
  3. customdried under reduced pressure
  4. additionTo the residue was added water
  5. extractionextracted with chloroform
  6. washThe extract was washed with water
  7. dry with materialbrine, and then dried over anhydrous magnesium sulfate
  8. customThe solvent was removed in vacuo
  9. additionA solution of the oily residue in DMF (5 ml) containing 4-(1-acetyl-4-piperidinylmethyl)-2-aminomethylmorpholine
  10. additionwas added to a reaction solution which
  11. customwas obtained
  12. stirringThe mixture was stirred at room temperature overnight
  13. extractionthe mixture was extracted with chloroform
  14. washthe extract was sequentially washed with saturated sodium bicarbonate, water and brine
  15. dry with materialdried over anhydrous magnesium sulfate
  16. customThe solvent was removed in vacuo
  17. customThe residue was purified by silica gel column chromatography (eluent: chloroform/methanol=30/1)

출처 및 근거

ORD 기록
ord-1f8f58481dbc4367b37209159634e29a
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07906510B2

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