Methanesulfonic Acid → HCID 67316404, 화합물

HRID 1013820

반응식

HRID 1013820 반응식
C([O:8][C:9]1[CH:30]=[C:29]([Cl:31])[C:12]([CH2:13][C@@H:14]2[CH2:18][CH2:17][N:16]([CH:19]3[C:27]4[NH:26][N:25]=[CH:24][C:23]=4[CH2:22][CH2:21][CH2:20]3)[C:15]2=[O:28])=[C:11]([Cl:32])[CH:10]=1)C1C=CC=CC=1.CS(O)(=O)=O>CSC>[Cl:31][C:29]1[CH:30]=[C:9]([OH:8])[CH:10]=[C:11]([Cl:32])[C:12]=1[CH2:13][C@@H:14]1[CH2:18][CH2:17][N:16]([CH:19]2[C:27]3[NH:26][N:25]=[CH:24][C:23]=3[CH2:22][CH2:21][CH2:20]2)[C:15]1=[O:28]

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 67316393(R)-3-(4-benzyloxy-2,6-dichloro-benzyl)-1-(4,5,6,7-tetrahydro-1H-indazol-7-yl)-pyrrolidin-2-one

생성물 1

HCID 67316404HCID 67316404, 화합물수율 110.6%

시약·촉매·용매 1

HCID 1068Dimethyl Sulfide용매

실험 절차

To a solution of (R)-3-(4-benzyloxy-2,6-dichloro-benzyl)-1-(4,5,6,7-tetrahydro-1H-indazol-7-yl)-pyrrolidin-2-one (2.46 g, 5.23 mmol) in dimethylsulfide (28 mL), add methane sulfonic acid (8.23 g, 85.7 mmol) and stir the mixture vigorously under at room temperature for 18 hours. Remove the solvent in vacuo and dilute the residue with water, adjust the pH to pH=7 with 5 N NaOH, and extract the mixture several times with ethyl acetate and THF. After drying the combined organic layer (Na2SO4), filter and concentrate under vacuum to afford 2.20 g (100%) of the title compound. MS (m/z): 381 (M+).

후처리

  1. customRemove the solvent in vacuo
  2. additiondilute the residue with water
  3. extractionextract the mixture several times with ethyl acetate and THF
  4. dry with materialAfter drying the combined organic layer (Na2SO4)
  5. filtrationfilter
  6. concentrationconcentrate under vacuum

출처 및 근거

ORD 기록
ord-18d1d8da0f5f4e8d83285295930e5853
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981918B2

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