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4-Formylbenzoic acid → HCID 59340335, 화합물

HRID 1643497
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HRID 1643497 반응식
[C:1]([C:4]1[CH:11]=[CH:10][C:7]([CH:8]=[O:9])=[CH:6][CH:5]=1)([OH:3])=O.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:36][CH2:37][CH2:38][N:39]1[CH2:44][CH2:43][CH:42]([O:45][C:46](=[O:60])[NH:47][C:48]2[CH:53]=[CH:52][CH:51]=[CH:50][C:49]=2[C:54]2[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=2)[CH2:41][CH2:40]1.CCN(C(C)C)C(C)C>C(Cl)Cl>[CH:8]([C:7]1[CH:10]=[CH:11][C:4]([C:1]([NH:36][CH2:37][CH2:38][N:39]2[CH2:44][CH2:43][CH:42]([O:45][C:46](=[O:60])[NH:47][C:48]3[CH:53]=[CH:52][CH:51]=[CH:50][C:49]=3[C:54]3[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=3)[CH2:41][CH2:40]2)=[O:3])=[CH:5][CH:6]=1)=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 120884-Formylbenzoic acidHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 53319786Biphenyl-2-ylcarbamic acid 1-(2-aminoethyl)piperidin-4-yl ester

생성물 1

HCID 59340335HCID 59340335, 화합물수율 92.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A mixture of 4-carboxybenzaldehyde (0.95 g, 6.35 mmol) and HATU (3.02 g, 7.94 mmol) in 55 mL of DCM was stirred at room temperature for 1 hour and then biphenyl-2-ylcarbamic acid 1-(2-aminoethyl)piperidin-4-yl ester (3 g, 5.29 mmol; prepared as described in Preparation 7) and DIPEA (4.6 mL, 26.45 mmol) were added. The resulting mixture was stirred at room temperature for 2 hours and then diluted with 100 mL of DCM and washed with saturated sodium bicarbonate (150 mL) and brine (150 mL). The organic layer was dried over MgSO4, filtered and concentrated to provide 2.3 g of the title intermediate (92% yield), which was suitable for use without further purification.

후처리

  1. stirringThe resulting mixture was stirred at room temperature for 2 hours
  2. washwashed with saturated sodium bicarbonate (150 mL) and brine (150 mL)
  3. dry with materialThe organic layer was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-db2c798141754b3398884d973b468c74
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08119796B2

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