Lithium iodide → HCID 20135083, 화합물

HRID 580408노트

반응식

HRID 580408 반응식
[I-].[Li+].COC([C:7]1([CH2:31][CH:32]=[CH2:33])[CH:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[O:20][CH3:21])[CH2:12][C:11]2[C:22]([C:26]([F:29])([F:28])[F:27])=[CH:23][CH:24]=[CH:25][C:10]=2[NH:9][C:8]1=[O:30])=O>N1C=CC=CC=1.O>[CH3:21][O:20][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[CH:13]1[CH2:12][C:11]2[C:22]([C:26]([F:27])([F:28])[F:29])=[CH:23][CH:24]=[CH:25][C:10]=2[NH:9][C:8](=[O:30])[CH:7]1[CH2:31][CH:32]=[CH2:33]

참가 물질

5

반응물 2

HCID 66321Lithium iodideHCID 20135070HCID 20135070, 화합물

생성물 1

HCID 20135083HCID 20135083, 화합물수율 69.9%

시약·촉매·용매 2

HCID 962Water촉매HCID 1049Pyridine용매2회

실험 절차

Lithium iodide (11.98 g; 89.44 mmole) was added to 1,3,4,5-tetrahydro-3-(methoxycarbonyl)-4-(methoxyphenyl)-3-(2-propenyl)-6-(trifluoromethyl)-2H-1-benzazepin-2-one (9.69 g; 22.36 mmole) in pyridine (40 ml) and water (a few drops). The mixture was refluxed with stirring for 11 hours. The pyridine was vacuum distilled off and the residue was dissolved into methanol and washed with 1N hydrochloric acid (three times), and saturated sodium chloride, and dried (magnesium sulfate). The concentrated residue was black indicating some decomposition occurred. The 9.67 g of this black residue was flash chromatographed (silica gel/3:1-hexane:ethyl acetate, followed by 1:1-hexane/ethyl acetate). Appropriate fractions were combined and concentrated giving 5.87 g of the title compound as a solid.

후처리

  1. temperatureThe mixture was refluxed
  2. distillationdistilled off
  3. dissolutionthe residue was dissolved into methanol
  4. washwashed with 1N hydrochloric acid (three times), and saturated sodium chloride
  5. dry with materialdried (magnesium sulfate)
  6. customchromatographed (silica gel/3:1-hexane:ethyl acetate, followed by 1:1-hexane/ethyl acetate)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-23cc770041854ba6ae44e2db714a5176
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04752645

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