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Water → HCID 23324574, 화합물

HRID 1380892
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HRID 1380892 반응식
[CH3:1][O:2][C:3]1[C:33]([O:34][CH3:35])=[CH:32][C:6]2[CH2:7][C:8](=[O:31])[N:9]([CH2:12][CH2:13][CH2:14][N:15]([CH3:30])[CH:16]3[CH2:25][CH2:24][C:23]4[C:18](=[CH:19][C:20]([O:28][CH3:29])=[C:21]([O:26][CH3:27])[CH:22]=4)[CH2:17]3)[CH2:10][CH2:11][C:5]=2[CH:4]=1.[Se](=O)=[O:37].O>O1CCOCC1>[CH3:1][O:2][C:3]1[C:33]([O:34][CH3:35])=[CH:32][C:6]2[C:7](=[O:37])[C:8](=[O:31])[N:9]([CH2:12][CH2:13][CH2:14][N:15]([CH3:30])[CH:16]3[CH2:25][CH2:24][C:23]4[C:18](=[CH:19][C:20]([O:28][CH3:29])=[C:21]([O:26][CH3:27])[CH:22]=4)[CH2:17]3)[CH2:10][CH2:11][C:5]=2[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24007Selenium DioxideHCID 13579649HCID 13579649, 화합물

생성물 1

HCID 23324574HCID 23324574, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Here, 1-[7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-[N-methyl-N-(6,7-dimethoxy-1,2,3,4-tetrahydronaphth-2-yl)-amino]-propane (1.64 g, 0.0034 mol) is added at 70° C. to a suspension of selenium dioxide (0.41 g, 0.0036 mol) and Celite (0.34 g) in 1,4-dioxan (17 ml) and water (0.68 ml) is added and the mixture is refluxed for 40 hours. After cooling, it is suction filtered, concentrated by rotary evaporation in vacuo and purified over silica gel (40 g) (32-63 μm) with methylene chloride and increasing amounts of ethanol (up to 40%). The clean fractions are concentrated by evaporation and the hydrochloride is precipitated from acetone. Yield: 0.6 g. Mp: >145° C. (decomp.).

후처리

  1. temperaturethe mixture is refluxed for 40 hours
  2. temperatureAfter cooling
  3. filtrationfiltered
  4. concentrationconcentrated by rotary evaporation in vacuo
  5. custompurified over silica gel (40 g) (32-63 μm) with methylene chloride
  6. temperatureincreasing amounts of ethanol (up to 40%)
  7. concentrationThe clean fractions are concentrated by evaporation
  8. customthe hydrochloride is precipitated from acetone

출처 및 근거

ORD 기록
ord-909aa004aced4a8aad892c7c58739f39
출처 데이터셋
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04584293

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