Potassium Carbonate → 3-[2-((R)-6,8-Dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenyl]-oxazolidine-2,4-dione

HRID 251872노트

반응식

HRID 251872 반응식
[C:1]([O:4][CH2:5][C:6](=[O:27])[NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C@H:14]1[C:23]2[C:18](=[C:19]([Cl:25])[CH:20]=[C:21]([Cl:24])[CH:22]=2)[CH2:17][N:16]([CH3:26])[CH2:15]1)(=[O:3])C.C(=O)([O-])[O-].[K+].[K+]>CO>[Cl:24][C:21]1[CH:22]=[C:23]2[C:18](=[C:19]([Cl:25])[CH:20]=1)[CH2:17][N:16]([CH3:26])[CH2:15][C@H:14]2[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=1[N:7]1[C:6](=[O:27])[CH2:5][O:4][C:1]1=[O:3]

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 59682852[2-((R)-6,8-Dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenyl-carbamoyl]methyl acetate

생성물 1

HCID 117180843-[2-((R)-6,8-Dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenyl]-oxazolidine-2,4-dione수율 92.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

[2-((R)-6,8-Dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenyl-carbamoyl]methyl acetate (180 mg) was dissolved in methanol (5 ml). With stirring, potassium carbonate (305 mg, finely powdered) was added and the mixture was then stirred efficiently at room temperature for 4 h. Subsequently, the solvent was evaporated off, and the residue was taken up in ethyl acetate and washed three times with water. The ethyl acetate phase was dried with magnesium sulfate, filtered and concentrated. 160 mg of the desired product were obtained.

후처리

  1. stirringthe mixture was then stirred efficiently at room temperature for 4 h
  2. customSubsequently, the solvent was evaporated off
  3. washwashed three times with water
  4. dry with materialThe ethyl acetate phase was dried with magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-6c393ce93aae4bb58c583c04b60453a1
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07868003B2

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