Hydrochloric Acid → 1,2-Dihydro-N-(2,4-difluorophenyl)-1-oxopyrrolo[3,2,1-kl]phenothiazine-2-carboxamide

HRID 54924

反応式

HRID 54924 の反応式
[H-].[Na+].[C:3]1(=O)C2[C:7]([S:8][C:9]3[C:14](N=2)=[CH:13][CH:12]=[CH:11][CH:10]=3)=[CH:6][CH:5]=[CH:4]1.[F:18][C:19]1[CH:24]=[C:23]([F:25])[CH:22]=[CH:21][C:20]=1[N:26]=[C:27]=[O:28].Cl.[CH3:30][N:31]([CH:33]=[O:34])[CH3:32]>>[F:18][C:19]1[CH:24]=[C:23]([F:25])[CH:22]=[CH:21][C:20]=1[NH:26][C:27]([CH:14]1[C:13]2[CH:12]=[CH:11][CH:10]=[C:9]3[S:8][C:7]4[CH:6]=[CH:5][CH:4]=[CH:3][C:32]=4[N:31]([C:30]=23)[C:33]1=[O:34])=[O:28]

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 5932582,4-Difluorophenyl isocyanateHCID 12998954Phenothiazine-1-one

生成物 1

HCID 144599751,2-Dihydro-N-(2,4-difluorophenyl)-1-oxopyrrolo[3,2,1-kl]phenothiazine-2-carboxamide

実験手順

To a suspension of sodium hydride (0.14 g) in DMF (10 ml) was added pyrrolo[3,2, -1kl]phenothiazine-1-one (0.48 g) and to the resulting solution was slowly added 2,4-difluorophenyl isocyanate (0.31 g). The reaction mixture was stirred for 12 hours and then poured onto ice water (50 ml). The resulting mixture was acidified to pH 2.0 with 6N HCl and the precipitated solid was collected and then air dried to yield the title compound (2.84 g). A sample recrystallized from methylene chloride had a m.p. of 208°-209° C.

後処理

  1. additionwas added pyrrolo[3,2
  2. additionpoured onto ice water (50 ml)
  3. customthe precipitated solid was collected
  4. customair dried

出典と根拠

ORDレコード
ord-87d4a85ef58a4c068d58b770ac1551a7
出典データセット
uspto-grants-1997_04
特許番号
US05624929

関連ノート

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