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Sodium Carbonate → HCID 131718800, 화합물

HRID 52029
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HRID 52029 반응식
Cl[C:2]1[C:7]([C:8]#[N:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[NH2:10][C:11]1[C:16]2[CH2:17][CH2:18][O:19][C:15]=2[C:14]([C:20]([NH:22][C@H:23]2[CH2:28][CH2:27][N:26]([CH2:29][CH2:30][CH2:31][CH2:32][NH2:33])[CH2:25][C@H:24]2[O:34][CH3:35])=[O:21])=[CH:13][C:12]=1[Cl:36].C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O>[OH2:19].[NH2:10][C:11]1[C:16]2[CH2:17][CH2:18][O:19][C:15]=2[C:14]([C:20]([NH:22][C@H:23]2[CH2:28][CH2:27][N:26]([CH2:29][CH2:30][CH2:31][CH2:32][NH:33][C:2]3[C:7]([C:8]#[N:9])=[CH:6][CH:5]=[CH:4][N:3]=3)[CH2:25][C@H:24]2[O:34][CH3:35])=[O:21])=[CH:13][C:12]=1[Cl:36].[NH2:10][C:11]1[C:16]2[CH2:17][CH2:18][O:19][C:15]=2[C:14]([C:20]([NH:22][C@H:23]2[CH2:28][CH2:27][N:26]([CH2:29][CH2:30][CH2:31][CH2:32][NH:33][C:2]3[C:7]([C:8]#[N:9])=[CH:6][CH:5]=[CH:4][N:3]=3)[CH2:25][C@H:24]2[O:34][CH3:35])=[O:21])=[CH:13][C:12]=1[Cl:36]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 810792-ChloronicotinonitrileHCID 67704528cis-4-amino-N-[1-(4-aminobutyl)-3-methoxy-4-piperidinyl]-5-chloro-2,3-dihydro-7-benzofurancarboxamide

생성물 1

HCID 131718800HCID 131718800, 화합물수율 35.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

A mixture of 1.4 parts of 2-chloro-3-pyridinecarbonitrile, 3.2 parts of cis-4-amino-N-[1-(4-aminobutyl)-3-methoxy -4-piperidinyl]-5-chloro-2,3-dihydro-7-benzofurancarboxamide, 65.8 parts of N,N-dimethylformamide and 1.3 parts of sodium carbonate was stirred for 20 hours at 70° C. The solvent was evaporated and the residue was dissolved in trichloromethane. The organic layer was washed with water, dried, filtered and evaporated. The residue was purified by column chromatography (silica gel; CHCl3 /CH3OH(NH3)98:2). The eluent of the desired fraction was evaporated and the residue was crystallized from 2,2'-oxybispropane. The product was dried in vacuo at 60° C., yielding 1.44 parts (35.4%) of cis-4-amino-5-chloro-N-[1-[4-[(3-cyano-2-pyridinyl)-amino]butyl]-3-methoxy-4-piperidinyl]-2,3-dihydro-7-benzofurancarboxamide hemihydrate; mp. 129.7° C. (comp. 6).

후처리

  1. customThe solvent was evaporated
  2. dissolutionthe residue was dissolved in trichloromethane
  3. washThe organic layer was washed with water
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by column chromatography (silica gel; CHCl3 /CH3OH(NH3)98:2)
  8. customThe eluent of the desired fraction was evaporated
  9. customthe residue was crystallized from 2,2'-oxybispropane
  10. customThe product was dried in vacuo at 60° C.

출처 및 근거

ORD 기록
ord-845bc1ef200f4d7098c763399ef04796
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05616583

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