3-Fluorophenyl isocyanate → HCID 68654593, 화합물

HRID 448262노트

반응식

HRID 448262 반응식
[NH2:1][C:2]1[C:3]2[CH2:14][N:13]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[C:12]([CH3:23])([CH3:22])[C:4]=2[N:5]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[N:6]=1.[F:24][C:25]1[CH:26]=[C:27]([N:31]=[C:32]=[O:33])[CH:28]=[CH:29][CH:30]=1>C1COCC1>[F:24][C:25]1[CH:26]=[C:27]([NH:31][C:32]([NH:1][C:2]2[C:3]3[CH2:14][N:13]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[C:12]([CH3:22])([CH3:23])[C:4]=3[N:5]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[N:6]=2)=[O:33])[CH:28]=[CH:29][CH:30]=1

참가 물질

4

반응물 2

HCID 1230643-Fluorophenyl isocyanateHCID 573530855-tert-butyl 1-ethyl 3-amino-6,6-dimethylpyrrolo[3,4-c]pyrazole-1,5(4H,6H)-dicarboxylate

생성물 1

HCID 68654593HCID 68654593, 화합물수율 71.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

5-tert-Butyl 1-ethyl 3-amino-6,6-dimethyl-4,6-dihydropyrrolo[3,4-c]pyrazole-1,5-dicarboxylate (3.0 g, 9.24 mmol) was dissolved in anhydrous THF (50 ml), treated at room temperature with 3-fluorophenyl-isocyanate (1.4 g, 10.21 mmol, 1.1 eq) and stirred overnight. The following day the reaction mixture was evaporated, taken up with DCM and washed with brine. The organic phase was dried over sodium sulfate and evaporated to dryness. Purification by flash chromatography (CH2Cl2/MeOH 90/10) afforded 3.05 g (yield 71%) of the title compound.

후처리

  1. customThe following day the reaction mixture was evaporated
  2. washwashed with brine
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. customevaporated to dryness
  5. customPurification by flash chromatography (CH2Cl2/MeOH 90/10)

출처 및 근거

ORD 기록
ord-23a306a1afcb42f39193e765ecf0a0f9
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481585B2

반응 노트

불러오는 중…