Potassium Hydroxide → 3-(6,8-Dichloro-1,2,3,4-tetrahydro-2-methyl-4-isoquinolinyl)benzoic acid

HRID 1295435ノート

反応式

HRID 1295435 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([Cl:12])[CH:11]=1)[CH2:8][N:7]([CH3:13])[CH2:6][CH:5]2[C:14]1[CH:15]=[C:16]([CH:22]=[CH:23][CH:24]=1)[C:17]([O:19]CC)=[O:18].[OH-].[K+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([Cl:12])[CH:11]=1)[CH2:8][N:7]([CH3:13])[CH2:6][CH:5]2[C:14]1[CH:15]=[C:16]([CH:22]=[CH:23][CH:24]=1)[C:17]([OH:19])=[O:18]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 22386927HCID 22386927、化合物2 回

生成物 1

HCID 223868523-(6,8-Dichloro-1,2,3,4-tetrahydro-2-methyl-4-isoquinolinyl)benzoic acid収率 55.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3.3 g of ethyl 3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzoate (intermediate 4) were dissolved in 60 ml of methanol and admixed with 60 ml of 2 N KOH. After two hours at 50° C., the mixture was concentrated in vacuo and the residue partitioned between water and ether. The water phase was adjusted to a pH of approx. 6 using 2 N HCl and the precipitate which formed was filtered off with suction. Drying afforded 1.7 g of the title compound as a colorless solid.

後処理

  1. concentrationthe mixture was concentrated in vacuo
  2. customthe residue partitioned between water and ether
  3. customthe precipitate which formed
  4. filtrationwas filtered off with suction
  5. customDrying

出典と根拠

ORDレコード
ord-21bda20232d3408d9cceef1a6cbc49bb
出典データセット
uspto-grants-2007_07
特許番号
US07241775B2

反応ノート

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