HCID 21715954、化合物 → HCID 86755326、化合物

HRID 1004526ノート

反応式

HRID 1004526 の反応式
CC(C)C[O:4][C:5](=[O:16])[CH2:6][CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][CH:10]=1.[C:18]([CH2:21][NH:22][C:23]1[C:24]([I:39])=[C:25]([C:29]([I:38])=[C:30]([NH:33][CH2:34][C:35](=[O:37])[CH3:36])[C:31]=1[I:32])[C:26](Cl)=[O:27])(=[O:20])[CH3:19]>CC(N(C)C)=O>[C:35]([CH2:34][NH:33][C:30]1[C:29]([I:38])=[C:25]([C:26]([NH:15][C:12]2[CH:11]=[CH:10][C:9]([CH2:8][CH2:7][CH2:6][C:5]([OH:4])=[O:16])=[CH:14][CH:13]=2)=[O:27])[C:24]([I:39])=[C:23]([NH:22][CH2:21][C:18](=[O:20])[CH3:19])[C:31]=1[I:32])(=[O:37])[CH3:36]

参加物

4

反応物 2

HCID 21715954HCID 21715954、化合物HCID 53982003HCID 53982003、化合物

生成物 1

HCID 86755326HCID 86755326、化合物収率 74%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
92.5 °C

実験手順

To a solution of 4-aminobenzenebutyric acid 2,2-dimethylethyl ester IXb (2.0 g, 7.5 mmol) in dimethylacetamide (DMA 25 mL), was added 3,5 bis(acetylmethylamino)-2,4,6 triiodobenzoyl chloride X (1.98 g, 3 mmol), and the mixture stirred at 90-95° C. for 6 h. The solvent was removed in vacuo and the residue was dissolved in ethyl acetate (200 mL). The organic extract was washed with saturated sodium bicarbonate (250 mL), water and saturated sodium chloride and dried over sodium sulfate. The solvent was removed in vacuum and the residue purified by a silica gel column (150 g) using hexane/EtOAc to obtain the title compound XIb (1.98 g, yield 74%). (MS: m/e 858 (M-H)-.

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in ethyl acetate (200 mL)
  3. extractionThe organic extract
  4. washwas washed with saturated sodium bicarbonate (250 mL), water and saturated sodium chloride
  5. dry with materialdried over sodium sulfate
  6. customThe solvent was removed in vacuum
  7. customthe residue purified by a silica gel column (150 g)

出典と根拠

ORDレコード
ord-9401cf15dfab4a9aabb19f3ea8c8fe00
出典データセット
uspto-grants-2000_04
特許番号
US06051210

反応ノート

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