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

HRID 251872ノート

反応式

HRID 251872 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

[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.

後処理

  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

出典と根拠

ORDレコード
ord-6c393ce93aae4bb58c583c04b60453a1
出典データセット
uspto-grants-2011_01
特許番号
US07868003B2

反応ノート

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