Hydrochloric Acid → HCID 46937305, 화합물

HRID 1926582노트

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HRID 1926582 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[C:18]([NH:20][S:21]([C:24]3[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH:31]([F:33])[F:32])[CH:25]=3)(=[O:23])=[O:22])[CH:17]=[CH:16][C:15]=2[CH3:34])[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:35]>ClCCl.C(OCC)C>[ClH:35].[F:33][CH:31]([F:32])[O:30][C:26]1[CH:25]=[C:24]([S:21]([NH:20][C:18]2[CH:17]=[CH:16][C:15]([CH3:34])=[C:14]([N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)[CH:19]=2)(=[O:22])=[O:23])[CH:29]=[CH:28][CH:27]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 665998364-[5-(3-Difluoromethoxy-benzenesulfonylamino)-2-methyl-phenyl]-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 46937305HCID 46937305, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

4-[5-(3-Difluoromethoxy-benzenesulfonylamino)-2-methyl-phenyl]-piperazine-1-carboxylic acid tert-butyl ester (0.097 g, 0.195 mmol) was dissolved in 5 mL of dichloromethane. A solution of 0.293 mL of 2N hydrochloric acid in diethyl ether was added and the mixture stirred for 16 h at room temperature. The solvents were evaporated, the residue purified via reversed phase HPLC and fractions containing the product were combined. The pH was adjusted to 9 with aqueous sodium bicarbonate and the aqueous layer extracted with dichloromethane. The organic phase was then dried over magnesium sulphate, filtered and evaporated to dryness. The residue was treated with a solution 2N hydrochloric acid in diethyl ether and the mixture evaporated to dryness to yield the title compound (0.017 mg).

후처리

  1. customThe solvents were evaporated
  2. customthe residue purified via reversed phase HPLC and fractions
  3. additioncontaining the product
  4. extractionthe aqueous layer extracted with dichloromethane
  5. dry with materialThe organic phase was then dried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated to dryness
  8. additionThe residue was treated with a solution 2N hydrochloric acid in diethyl ether
  9. customthe mixture evaporated to dryness

출처 및 근거

ORD 기록
ord-f2e20cd6da63464ea2e9c6762fa0052f
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183237B2

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