Phosphoric Acid → HCID 178518347, 화합물

HRID 2236800노트

반응식

HRID 2236800 반응식
[I:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[NH:7][C:6](=[O:13])/[C:5]/2=[CH:14]\[NH:15][C:16]1[CH:21]=[CH:20][C:19]([N:22]2[CH2:27][CH2:26][N:25](C(OC(C)(C)C)=O)[CH2:24][CH2:23]2)=[CH:18][CH:17]=1.P(=O)(O)(O)O>CN(C)C=O>[I:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[NH:7][C:6](=[O:13])/[C:5]/2=[CH:14]\[NH:15][C:16]1[CH:17]=[CH:18][C:19]([N:22]2[CH2:23][CH2:24][NH:25][CH2:26][CH2:27]2)=[CH:20][CH:21]=1

참가 물질

4

반응물 2

HCID 1004Phosphoric AcidHCID 178452239HCID 178452239, 화합물

생성물 1

HCID 178518347HCID 178518347, 화합물수율 24.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A N,N-dimethylformamide mixture (0.6 mL) of tert-butyl 4-(4-{[(Z)-(6-iodo-1,3-dioxo-2,3-dihydroisoquinolin-4(1H)-ylidene)methyl]amino}phenyl)piperazine-1-carboxylate (50 mg, 0.087 mmol) and concentrated phosphoric acid (0.6 mL) is heated at 60 C for 2 h. After evaporating to dryness, the residue is partitioned between methylene chloride and saturated sodium bicarbonate. The organic layer is washed with water, dried, and evaporated to yield 10 mg (24%) of the title compound as an orange solid. MS (ESI) m/z 475.2 (M+H)+1

후처리

  1. customAfter evaporating to dryness
  2. customthe residue is partitioned between methylene chloride and saturated sodium bicarbonate
  3. washThe organic layer is washed with water
  4. customdried
  5. customevaporated

출처 및 근거

ORD 기록
ord-216c8b4dbb024ab2a5582657fd9dcd00
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

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