Phosphoric Acid → HCID 178518347、化合物

HRID 2236800ノート

反応式

HRID 2236800 の反応式
[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

参加物

4

反応物 2

HCID 1004Phosphoric AcidHCID 178452239HCID 178452239、化合物

生成物 1

HCID 178518347HCID 178518347、化合物収率 24.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-216c8b4dbb024ab2a5582657fd9dcd00
出典データセット
uspto-grants-2010_05
特許番号
US07713994B2

反応ノート

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