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

HRID 54924

반응식

HRID 54924 반응식
[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]

참가 물질

6

반응물 5

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

생성물 1

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

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-87d4a85ef58a4c068d58b770ac1551a7
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624929

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