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Hydrochloric Acid → HCID 178526950, 화합물

HRID 1004414
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HRID 1004414 반응식
[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:17]=[CH:16][C:15](Br)=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:19][C:20]1[C:29]2[O:28][C:27]([C:30]3[NH:34][N:33]=[N:32][N:31]=3)=[CH:26][C:25](=[O:35])[C:24]=2[CH:23]=[CH:22][CH:21]=1.N12CCCN=C1CCCCC2.Cl.[C:48]([O-])(=[O:50])C.[Na+]>CN1CCCC1=O.O.CO.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl>[OH2:11].[O:35]=[C:25]1[C:24]2[CH:23]=[CH:22][CH:21]=[C:20]([NH:19][C:48](=[O:50])[C:15]3[CH:16]=[CH:17][C:12]([O:11][CH2:10][CH2:9][CH2:8][CH2:7][C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)=[CH:13][CH:14]=3)[C:29]=2[O:28][C:27]([C:30]2[NH:34][N:33]=[N:32][N:31]=2)=[CH:26]1.[O:35]=[C:25]1[C:24]2[CH:23]=[CH:22][CH:21]=[C:20]([NH:19][C:48](=[O:50])[C:15]3[CH:16]=[CH:17][C:12]([O:11][CH2:10][CH2:9][CH2:8][CH2:7][C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)=[CH:13][CH:14]=3)[C:29]=2[O:28][C:27]([C:30]2[NH:34][N:33]=[N:32][N:31]=2)=[CH:26]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 517045Sodium AcetateHCID 108704574-(4-Phenylbutoxy)bromobenzeneHCID 178507421HCID 178507421, 화합물

생성물 1

HCID 178526950HCID 178526950, 화합물수율 78.7%

시약·촉매·용매 4

HCID 6102075Dichlorobis(triphenylphosphine)palladium촉매HCID 887Methanol용매HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

A mixture of 4-(4-phenylbutoxy)bromobenzene (0.50 g, 1.64 mmole), 8-amino-4-oxo-2-(tetrazol-5-yl)-4H-1-benzopyran (0.75 g, 3.28 mmole), bis-(triphenylphospine)palladium (II) chloride (0.135 g, 0.19 mmole) and 1,8-diazabicyclo[5.4.0]undec-7-ene (0.87 g, 5.74 mmole) was stirred in N-methylpyrrolidinone (10 ml) at 100-110° C. under an atmosphere of carbon monoxide at atmospheric pressure for 4.5 hours. The reaction mixture was diluted with water (15 ml) and acidified using concentrated hydrochloric acid (5 ml). The precipitate was filtered, washed with water and methanol and then stirred in concentrated hydrochloric acid (8 ml) to dissolve unreacted 8-amino-4-oxo-2-(tetrazol-5-yl)-4H-1-benzopyran. The undissolved solid was filtered, washed with concentrated hydrochloric (2×1.5 ml), water, then methanol. The damp cake was stirred with sodium acetate (0.15 g, 1.83 mmole) in methanol (10 ml) and the solution filtered. The supernatant liquor was acidified with concentrated hydrochloric acid (0.2 ml), and the product filtered, washed with methanol and dried to give the title compound (422 mg, 53%).

후처리

  1. filtrationThe precipitate was filtered
  2. washwashed with water and methanol
  3. dissolutionto dissolve unreacted 8-amino-4-oxo-2-(tetrazol-5-yl)-4H-1-benzopyran
  4. filtrationThe undissolved solid was filtered
  5. washwashed
  6. concentrationwith concentrated hydrochloric (2×1.5 ml), water
  7. filtrationthe solution filtered
  8. filtrationthe product filtered
  9. washwashed with methanol
  10. customdried

출처 및 근거

ORD 기록
ord-20dfe70612ba4bf2a79bedfcee9a97cc
출처 데이터셋
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06048983

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