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Acetic Acid → HCID 70873377、化合物

HRID 2172258
ノート
印刷プレビュー

反応式

HRID 2172258 の反応式
[N+:1]([C:4]1[N:5]=[C:6]2[N:11]([CH:12]=1)[CH2:10][CH2:9][C@H:8]([CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([N:21]3[CH2:26][CH2:25][C:24](=O)[CH2:23][CH2:22]3)=[CH:17][CH:16]=1)[O:7]2)([O-:3])=[O:2].[F:28][C:29]([F:46])([F:45])[O:30][C:31]1[CH:44]=[CH:43][C:34]([O:35][C:36]2[CH:41]=[CH:40][C:39]([NH2:42])=[CH:38][CH:37]=2)=[CH:33][CH:32]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(O)(=O)C>ClCCCl.O1CCCC1>[N+:1]([C:4]1[N:5]=[C:6]2[N:11]([CH:12]=1)[CH2:10][CH2:9][C@H:8]([CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([N:21]3[CH2:22][CH2:23][CH:24]([NH:42][C:39]4[CH:40]=[CH:41][C:36]([O:35][C:34]5[CH:43]=[CH:44][C:31]([O:30][C:29]([F:28])([F:45])[F:46])=[CH:32][CH:33]=5)=[CH:37][CH:38]=4)[CH2:25][CH2:26]3)=[CH:17][CH:16]=1)[O:7]2)([O-:3])=[O:2]
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 176Acetic AcidHCID 5049666Sodium triacetoxyborohydrideHCID 116661924-(4-(Trifluoromethoxy)phenoxy)anilineHCID 70874615HCID 70874615、化合物

生成物 1

HCID 70873377HCID 70873377、化合物収率 19.2%

試薬・触媒・溶媒 2

HCID 11
1,2-Dichloroethane
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

1-[4-((R)-2-Nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazin-7-ylmethoxy)phenyl]piperidin-4-one (700 mg) and 4-(4-trifluoromethoxyphenoxy)phenylamine (557 mg) were suspended in 1,2-dichloroethane (20 ml) and tetrahydrofuran (20 ml). Sodium triacetoxyborohydride (558 mg) and acetic acid (0.13 ml) were added to the suspension, and stirred at room temperature for 20 hours. The reaction mixture was concentrated under reduced pressure and the remaining water layer was ice-cooled. A 20% sodium carbonate aqueous solution was added thereto, followed by extraction with methylene chloride. The organic layer was washed with a saturated sodium chloride aqueous solution and dried over sodium sulfate. After filtering, the filtrate was concentrated under reduced pressure. The residue was then purified by silica gel column chromatography (methylene chloride:methanol=100:1→methylene chloride:methanol=40:1) and recrystallized from isopropyl alcohol-isopropyl ether to afford the title compound as a yellow solid (226 mg).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. temperaturecooled
  3. additionA 20% sodium carbonate aqueous solution was added
  4. extractionfollowed by extraction with methylene chloride
  5. washThe organic layer was washed with a saturated sodium chloride aqueous solution
  6. dry with materialdried over sodium sulfate
  7. filtrationAfter filtering
  8. concentrationthe filtrate was concentrated under reduced pressure
  9. customThe residue was then purified by silica gel column chromatography (methylene chloride:methanol=100:1→methylene chloride:methanol=40:1)
  10. customrecrystallized from isopropyl alcohol-isopropyl ether

出典と根拠

ORDレコード
ord-2eefdb16d8a042d39c2e6f2b7b23aa06
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09051333B2

反応ノート

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