Hydrochloric Acid → HCID 58028470、化合物

HRID 42386ノート

反応式

HRID 42386 の反応式
[O:1]1CCO[CH:2]1[C:6]1[CH:7]=[C:8]([N:12]([C:50]2[C:59]3[C:54](=[CH:55][CH:56]=[CH:57][CH:58]=3)[CH:53]=[CH:52][CH:51]=2)[C:13]2[CH:25]=[CH:24][C:23]3[C:22]4[C:17](=[CH:18][C:19]([N:26]([C:37]5[CH:42]=[CH:41][CH:40]=[C:39]([CH:43]6OCC[O:44]6)[CH:38]=5)[C:27]5[C:36]6[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=6)[CH:30]=[CH:29][CH:28]=5)=[CH:20][CH:21]=4)[C:16]([CH3:49])([CH3:48])[C:15]=3[CH:14]=2)[CH:9]=[CH:10][CH:11]=1.Cl>CC(C)=O>[CH3:48][C:16]1([CH3:49])[C:17]2[CH:18]=[C:19]([N:26]([C:37]3[CH:38]=[C:39]([CH:40]=[CH:41][CH:42]=3)[CH:43]=[O:44])[C:27]3[C:36]4[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:30]=[CH:29][CH:28]=3)[CH:20]=[CH:21][C:22]=2[C:23]2[C:15]1=[CH:14][C:13]([N:12]([C:8]1[CH:7]=[C:6]([CH:11]=[CH:10][CH:9]=1)[CH:2]=[O:1])[C:50]1[C:59]3[C:54](=[CH:55][CH:56]=[CH:57][CH:58]=3)[CH:53]=[CH:52][CH:51]=1)=[CH:25][CH:24]=2

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58028464N2,N7-bis(3-(1,3-dioxolan-2-yl)phenyl)-9,9-dimethyl-N2,N7-di(naphthalen-1-yl)-9H-fluorene-2,7-diamine

生成物 1

HCID 58028470HCID 58028470、化合物収率 97.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a three-neck round-bottom flask, were added 8.0 g N2,N7-bis(3-(1,3-dioxolan-2-yl)phenyl)-9,9-dimethyl-N2,N7-di(naphthalen-1-yl)-9H-fluorene-2,7-diamine and in 100 mL acetone. 41.1 mL 2 M hydrochloric acid solution was added slowly to the reaction mixture through an addition funnel. After TLC showed the reaction was done, the solvent was removed by evaporation. 200 mL Ethyl acetate was added, and the reaction mixture was extracted using DI water (4×200 mL). The organic layer was dried over sodium sulfate. After filtration, the solvent was removed by evaporation. The product (6.9 g) was obtained after drying under vacuum, and was carried on to next step without further purification. The structure was confirmed by NMR.

後処理

  1. customthe solvent was removed by evaporation
  2. addition200 mL Ethyl acetate was added
  3. extractionthe reaction mixture was extracted
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. filtrationAfter filtration
  6. customthe solvent was removed by evaporation

出典と根拠

ORDレコード
ord-fafe8098a9f844e38edafb69aafdbaef
出典データセット
uspto-grants-2013_09
特許番号
US08535974B2

反応ノート

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