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Tetrahydrofuran → HCID 18545432, 화합물

HRID 564867
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HRID 564867 반응식
C1C[O:4][CH2:3]C1.Cl[C:7]1[N:12]=[C:11]([N:13]2[C:17]([CH3:18])=[C:16](/[CH:19]=[CH:20]/[CH2:21][N:22]3[CH2:27][CH2:26][N:25]([C:28]4[CH:33]=[C:32]([F:34])[CH:31]=[C:30]([F:35])[CH:29]=4)[CH2:24][CH2:23]3)[CH:15]=[N:14]2)[CH:10]=[C:9]([CH3:36])[N:8]=1.CO[C:39]1[CH:46]=[CH:45][C:42]([CH2:43][NH2:44])=[CH:41][CH:40]=1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)Cl>[F:35][C:30]1[CH:29]=[C:28]([N:25]2[CH2:26][CH2:27][N:22]([CH2:21]/[CH:20]=[CH:19]/[C:16]3[CH:15]=[N:14][N:13]([C:11]4[CH:10]=[C:9]([CH3:36])[N:8]=[C:7]([NH:44][CH2:43][C:42]5[CH:41]=[CH:40][CH:39]=[CH:46][C:45]=5[O:4][CH3:3])[N:12]=4)[C:17]=3[CH3:18])[CH2:23][CH2:24]2)[CH:33]=[C:32]([F:34])[CH:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 754524-MethoxybenzylamineHCID 18545346HCID 18545346, 화합물

생성물 1

HCID 18545432HCID 18545432, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To 15 ml of a THF solution of 155 mg of the compound obtained in Example 35 were added 240 mg of p-methoxybenzylamine and 50 mg (0.362 mmol) of potassium carbonate, followed by refluxing for 60 hours. Chloroform was added to the reaction mixture, and the mixture was washed with a saturated sodium chloride aqueous solution. The combined organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated. The residue was subjected to silica gel column chromatography using a 99:1 mixture (by volume) of chloroform and methanol as a developing solution. The fraction containing the desired compound was concentrated to give 183 mg of the title compound.

후처리

  1. temperatureby refluxing for 60 hours
  2. washthe mixture was washed with a saturated sodium chloride aqueous solution
  3. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated
  5. additionThe fraction containing the desired compound
  6. concentrationwas concentrated

출처 및 근거

ORD 기록
ord-98920d4eb731462887356aeca375528a
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06169086A

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