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Sodium Iodide → HCID 86709401、化合物

HRID 2172266
ノート
印刷プレビュー

反応式

HRID 2172266 の反応式
C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].FC(F)(F)C(O)=O.[CH3:16][C@H:17]1[CH2:22][NH:21][C@H:20]([CH3:23])[CH2:19][N:18]1[C:24]1[CH:43]=[CH:42][C:27]([O:28][CH2:29][C@@H:30]2[O:35][C:34]3=[N:36][C:37]([N+:39]([O-:41])=[O:40])=[CH:38][N:33]3[CH2:32][CH2:31]2)=[CH:26][CH:25]=1.Cl[CH2:45][C:46]1[CH:51]=[CH:50][C:49]([O:52][C:53]2[CH:58]=[CH:57][C:56]([O:59][C:60]([F:63])([F:62])[F:61])=[CH:55][CH:54]=2)=[CH:48][CH:47]=1.CC(C)([O-])C.[Na+]>O.CN1CCCC1=O>[CH3:16][C@H:17]1[CH2:22][N:21]([CH2:45][C:46]2[CH:47]=[CH:48][C:49]([O:52][C:53]3[CH:58]=[CH:57][C:56]([O:59][C:60]([F:61])([F:62])[F:63])=[CH:55][CH:54]=3)=[CH:50][CH:51]=2)[C@H:20]([CH3:23])[CH2:19][N:18]1[C:24]1[CH:25]=[CH:26][C:27]([O:28][CH2:29][C@@H:30]2[O:35][C:34]3=[N:36][C:37]([N+:39]([O-:41])=[O:40])=[CH:38][N:33]3[CH2:32][CH2:31]2)=[CH:42][CH:43]=1
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

8

反応物 5

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 222930671-(Chloromethyl)-4-[4-(trifluoromethoxy)phenoxy]benzeneHCID 23676156Sodium t-butoxideHCID 86709402HCID 86709402、化合物

生成物 1

HCID 86709401HCID 86709401、化合物

試薬・触媒・溶媒

2
HCID 962Water溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
60 °C

実験手順

Potassium carbonate (135 mg) and sodium iodide (146 mg) were added to an N-methylpyrrolidone solution (6 ml) of (R)-7-[4-((2S,5R)-2,5-dimethyl-piperazin-1-yl)phenoxymethyl]-2-nitro-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazine trifluoroacetate (343 mg) and 1-(chloromethyl)-4-[4-(trifluoromethoxy)phenoxy]benzene (269 mg), and the mixture was stirred at 60° C. for 3 hours. Sodium tert-butoxide (112 mg) was added to the mixture and stirred at room temperature for 3 hours. Water was added thereto, followed by extraction with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution and then dried over sodium sulfate. After filtering, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:1→ethyl acetate:n-hexane=3:1) to afford the title compound as a pale brown amorphous compound (200 mg).

後処理

  1. stirringstirred at room temperature for 3 hours
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe organic layer was washed with a saturated sodium chloride aqueous solution
  4. dry with materialdried over sodium sulfate
  5. filtrationAfter filtering
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:1→ethyl acetate:n-hexane=3:1)

出典と根拠

ORDレコード
ord-d179a5e3a6e64c16a24e8f0af8d40122
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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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート