Sodium Thiosulfate → HCID 69700183, 화합물

HRID 1061007노트

반응식

HRID 1061007 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][N:22]([C:25](=[O:38])[C:26]2[CH:31]=[CH:30][C:29]([C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][N:33]=3)=[CH:28][CH:27]=2)[CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].S([O-])([O-])(=O)=S.[Na+].[Na+]>ClCCl>[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][N:22]([C:25]([C:26]2[CH:31]=[CH:30][C:29]([C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][N+:33]=3[O-:9])=[CH:28][CH:27]=2)=[O:38])[CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:13])[CH3:14]

참가 물질

5

반응물 3

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 22709582HCID 22709582, 화합물

생성물 1

HCID 69700183HCID 69700183, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

At −10° C., metachloroperbenzoic acid (789 mg) was added to a solution of 1-tert-butoxycarbonyl-4-[4-(2-pyridyl)benzoyl]piperazine (517 mg) in dichloromethane (dichloromethane: 8 ml). The resulting mixture was stirred for 24 hours, followed by dilution with dichloromethane. A small amount of an aqueous sodium thiosulfate solution and saturated saline were added to the dilute solution. The organic layer so separated was washed with a saturated aqueous solution of sodium bicarbonate and saturated saline and then dried over anhydrous sodium sulfate. The residue obtained by distilling off the solvent under reduced pressure was purified by chromatography on a silica gel column (dichloromethane:methanol=20:1), whereby the title compound (415 mg, 77%) was obtained.

후처리

  1. customThe organic layer so separated
  2. washwas washed with a saturated aqueous solution of sodium bicarbonate and saturated saline
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe residue obtained
  5. distillationby distilling off the solvent under reduced pressure
  6. customwas purified by chromatography on a silica gel column (dichloromethane:methanol=20:1), whereby the title compound (415 mg, 77%)
  7. customwas obtained

출처 및 근거

ORD 기록
ord-ccb0bcc52bc64c6eb51f051e6544c7cc
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525042B1

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