HCID 21715954, 화합물 → HCID 86755326, 화합물

HRID 1004526노트

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HRID 1004526 반응식
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]

참가 물질

4

반응물 2

HCID 21715954HCID 21715954, 화합물HCID 53982003HCID 53982003, 화합물

생성물 1

HCID 86755326HCID 86755326, 화합물수율 74%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

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온도
92.5 °C

실험 절차

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)-.

후처리

  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)

출처 및 근거

ORD 기록
ord-9401cf15dfab4a9aabb19f3ea8c8fe00
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06051210

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