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Hydrochloric Acid → HCID 178526950、化合物

HRID 1004414
ノート
印刷プレビュー

反応式

HRID 1004414 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

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

生成物 1

HCID 178526950HCID 178526950、化合物収率 78.7%

試薬・触媒・溶媒

4
HCID 6102075Dichlorobis(triphenylphosphine)palladium触媒HCID 887Methanol溶媒HCID 962Water溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-20dfe70612ba4bf2a79bedfcee9a97cc
出典データセット
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06048983

反応ノート

読み込み中…

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