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

HRID 1295435노트

반응식

HRID 1295435 반응식
[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]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 22386927HCID 22386927, 화합물2회

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-21bda20232d3408d9cceef1a6cbc49bb
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07241775B2

반응 노트

불러오는 중…