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Hydrochloric Acid → 6-(4-{[(5-(1-Methylethyl)-3-{[(2,4,6-trifluorophenyl)oxy]methyl}-4-isoxazolyl)methyl]oxy}phenyl)-2-quinolinecarboxylic acid

HRID 2423462
ノート
印刷プレビュー

反応式

HRID 2423462 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([F:9])[C:3]=1[OH:10].O[CH2:12][C:13]1[C:17]([CH2:18][O:19][C:20]2[CH:25]=[CH:24][C:23]([C:26]3[CH:27]=[C:28]4[C:33](=[CH:34][CH:35]=3)[N:32]=[C:31]([C:36]([O:38]C)=[O:37])[CH:30]=[CH:29]4)=[CH:22][CH:21]=2)=[C:16]([CH:40]([CH3:42])[CH3:41])[O:15][N:14]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OC(C)C)=O)=NC(OC(C)C)=O.[OH-].[Na+].Cl>ClCCl.O1CCCC1.O.CO>[CH3:42][CH:40]([C:16]1[O:15][N:14]=[C:13]([CH2:12][O:10][C:3]2[C:2]([F:1])=[CH:7][C:6]([F:8])=[CH:5][C:4]=2[F:9])[C:17]=1[CH2:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]2[CH:27]=[C:28]3[C:33](=[CH:34][CH:35]=2)[N:32]=[C:31]([C:36]([OH:38])=[O:37])[CH:30]=[CH:29]3)=[CH:22][CH:21]=1)[CH3:41]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

11

反応物 6

HCID 313Hydrochloric AcidHCID 11776TriphenylphosphineHCID 14798Sodium HydroxideHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 5199742,4,6-TrifluorophenolHCID 59321462Methyl 6-[4-({[3-(hydroxymethyl)-5-(1-methylethyl)-4-isoxazolyl]methyl}oxy)phenyl]-2-quinolinecarboxylate

生成物 1

HCID 59321490
6-(4-{[(5-(1-Methylethyl)-3-{[(2,4,6-trifluorophenyl)oxy]methyl}-4-isoxazolyl)methyl]oxy}phenyl)-2-quinolinecarboxylic acid
収率 36.5%

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
100 °C

実験手順

To a solution of 2,4,6-trifluorophenol (18 mg, 0.12 mmol), methyl 6-[4-({[3-(hydroxymethyl)-5-(1-methylethyl)-4-isoxazolyl]methyl}oxy)phenyl]-2-quinoline carboxylate (52 mg, 0.12 mmol) and triphenylphosphine (35 mg, 0.13 mmol) in dichloromethane (2 mL) was added diisopropyl azodicarboxylate (0.024 mL, 0.13 mmol) slowly. The solution was heated in a microwave reactor at 100° C. for 10 minutes. The solution was adsorbed onto silica gel and purification was done by chromatography (0-70% ethyl acetate in hexanes) to afford a solid which was dissolved in 2:1 tetrahydrofuran:methanol (1.5 mL). Then 1 N sodium hydroxide (0.19 mmol, 0.19 mmol) was added. The solution was subjected to microwave radiation at 120° C. for 500 seconds. The solution was concentrated then diluted with water before the addition of 1 N hydrochloric acid (0.19 mmol, 0.19 mmol). The resulting solid was extracted with ethyl acetate twice and the combined organic layers were dried over magnesium sulfate and concentrated. The resulting solid was washed with methanol and dried to afford 6-(4-{[(5-(1-methylethyl)-3-{[(2,4,6-trifluorophenyl)oxy]methyl}-4-isoxazolyl)methyl]oxy}phenyl)-2-quinolinecarboxylic acid (24 mg, 35%). 1H-NMR (400 MHz, DMSO-d6) δ 8.44-8.06 (m, 5H), 7.69 (d, J=9 Hz, 2H), 7.11 (d, J=9 Hz, 2H), 6.65 (t, J=9 Hz, 2H), 5.23 (s, 2H), 5.12 (s, 2H), 3.29 (septet, J=7 Hz, 1H), 1.37 (d, J=7 Hz, 6H). HRMS (ESI) C30H23F3N2O5 calculated: 549.1632 (M+H)+, found: 549.1631 (M+H)+.

後処理

  1. customThe solution was adsorbed onto silica gel and purification
  2. customto afford a solid which
  3. customat 120° C.
  4. customfor 500 seconds
  5. concentrationThe solution was concentrated
  6. extractionThe resulting solid was extracted with ethyl acetate twice
  7. dry with materialthe combined organic layers were dried over magnesium sulfate
  8. concentrationconcentrated
  9. washThe resulting solid was washed with methanol
  10. customdried

出典と根拠

ORDレコード
ord-5c4ffeb39ba1428e8a389e7ced810504
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07960552B2

反応ノート

読み込み中…

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