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Sodium Carbonate → 4-(1-Acetyl-1,2,3,4-tetrahydroquinolin-6-yl)-3-methylbenzoic acid

HRID 1870893
ノート
印刷プレビュー

反応式

HRID 1870893 の反応式
B([C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][C:5]=1[CH3:13])(O)O.[C:14]([N:17]1[C:26]2[C:21](=[CH:22][C:23](OS(C(F)(F)F)(=O)=O)=[CH:24][CH:25]=2)[CH2:20][CH2:19][CH2:18]1)(=[O:16])[CH3:15].[Cl-].[Li+].C(=O)([O-])[O-].[Na+].[Na+]>O.C(COC)OC>[C:14]([N:17]1[C:26]2[C:21](=[CH:22][C:23]([C:4]3[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][C:5]=3[CH3:13])=[CH:24][CH:25]=2)[CH2:20][CH2:19][CH2:18]1)(=[O:16])[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 10340Sodium CarbonateHCID 433294Lithium ChlorideHCID 186942601-Acetyl-1,2,3,4-tetrahydro-6-trifluoromethanesulphonyloxyquinolineHCID 221158924-Borono-3-methylbenzoic acid

生成物 1

HCID 186942454-(1-Acetyl-1,2,3,4-tetrahydroquinolin-6-yl)-3-methylbenzoic acid収率 104%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

4-Borono-3-methylbenzoic acid (D29) (220 mg, 1.2 mmol), 1-acetyl-1,2,3,4-tetrahydro-6-trifluoromethanesulphonyloxyquinoline (D41, 410 mg, 1.25 mmol), lithium chloride (150 mg, 3.6 mmol) and sodium carbonate (505 mg, 4.7 mmol) were dissolved in a mixture of water (10 ml) and dimethoxyethane (10 ml). The suspension was degassed with argon for 15 mins and then treated with tetrakis (triphenylphosphine)palladium (O) (68 mg). The reaction mixture was heated at reflux for 28 hrs, then concentrated in vacuo. The residue was treated with 10% aqueous Na2CO3 solution and washed with ethyl acetate. The aqueous layer was acidified with 5M HCl and the resultant precipitate was filtered off and dried to afford the title compound as a light brown solid (386 mg, 100%).

後処理

  1. customThe suspension was degassed with argon for 15 mins
  2. additiontreated with tetrakis (triphenylphosphine)palladium (O) (68 mg)
  3. temperatureThe reaction mixture was heated
  4. temperatureat reflux for 28 hrs
  5. concentrationconcentrated in vacuo
  6. additionThe residue was treated with 10% aqueous Na2CO3 solution
  7. washwashed with ethyl acetate
  8. filtrationthe resultant precipitate was filtered off
  9. customdried

出典と根拠

ORDレコード
ord-4ebc3f3663be43f89f1996dc74814d80
出典データセット
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06100272

反応ノート

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