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Iodine → HCID 470744, 화합물

HRID 724928
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HRID 724928 반응식
[CH2:1]([N:3]1[C:9]2[N:10]=[CH:11][C:12]([CH2:14][CH2:15][C:16]3[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=3)=[CH:13][C:8]=2[C:7](=[O:22])[N:6]([CH3:23])[C:5]2[CH:24]=[CH:25][C:26]([Sn](C)(C)C)=[N:27][C:4]1=2)[CH3:2].[I:32]I>C(Cl)(Cl)Cl>[CH2:1]([N:3]1[C:9]2[N:10]=[CH:11][C:12]([CH2:14][CH2:15][C:16]3[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=3)=[CH:13][C:8]=2[C:7](=[O:22])[N:6]([CH3:23])[C:5]2[CH:24]=[CH:25][C:26]([I:32])=[N:27][C:4]1=2)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 807IodineHCID 11800160HCID 11800160, 화합물

생성물 1

HCID 470744HCID 470744, 화합물수율 21%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

To a solution of 5,11-dihydro-11-ethyl-8-[2-(4-pyridyl)ethyl]-2-trimethylstannyl-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (47 mg, 0.09 mmol) in chloroform was added a solution of iodine in chloroform (0.1M, 4 mL, 0.4 mmol). After 24 hours, the reaction mixture was washed with saturated aqueous KF, 5% NaHSO3, and saturated aq. sodium chloride. Purification by flash chromatography (elution with methanol-dichloromethane) and recrystallization (ethyl acetate-hexanes) afforded 15 mg (21%) of the title compound, m.p. 174° C.

후처리

  1. washthe reaction mixture was washed with saturated aqueous KF, 5% NaHSO3, and saturated aq. sodium chloride
  2. customPurification
  3. washby flash chromatography (elution with methanol-dichloromethane) and recrystallization (ethyl acetate-hexanes)

출처 및 근거

ORD 기록
ord-732904582cf34f42a9c580a7c33b4fff
출처 데이터셋
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05705499

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