Water → HCID 10472106, 화합물

HRID 1358558노트

반응식

HRID 1358558 반응식
Br[CH:2]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][C:14]=2[Cl:16])[C:9](=[O:17])[C:8]2[C:7]([Cl:18])=[CH:6][CH:5]=[CH:4][C:3]1=2.C(=O)([O-])[O-].[Ca+2].[CH2:24]([OH:28])[CH:25]([CH3:27])[CH3:26].O>C1COCC1>[CH2:24]([O:28][CH:2]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][C:14]=2[Cl:16])[C:9](=[O:17])[C:8]2[C:7]([Cl:18])=[CH:6][CH:5]=[CH:4][C:3]1=2)[CH:25]([CH3:27])[CH3:26]

참가 물질

6

반응물 4

HCID 962WaterHCID 6560IsobutanolHCID 10112Calcium CarbonateHCID 12082572HCID 12082572, 화합물

생성물 1

HCID 10472106HCID 10472106, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of compound (6) (2.0 mmol) and anhydrous calcium carbonate (0.5 g) in dry THF (20 ml) was added dropwise a solution of an appropriate iso-butanol (10 ml) in dry THF (10 ml) under N2. The reaction mixture was refluxed for 3 hours. Water (250 ml) was added and then extracted with dichloromethane. The combined organic extracts were washed with water, dried (MgSO4), and concentrated. The resulting precipitate was collected by filtration, washed with water and further purified by crystallization (CH3CN).

후처리

  1. temperatureThe reaction mixture was refluxed for 3 hours
  2. extractionextracted with dichloromethane
  3. washThe combined organic extracts were washed with water
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. filtrationThe resulting precipitate was collected by filtration
  7. washwashed with water
  8. customfurther purified by crystallization (CH3CN)

출처 및 근거

ORD 기록
ord-75e11d97db0244fab874bff07d53ca93
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06596774B1

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