홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Hydrochloric Acid → 2-Butyl-3-oxo-2,3,5,6,7,8-hexahydroisoquinoline-4-carboxylic acid benzylamide

HRID 489291
노트
인쇄 미리보기

반응식

HRID 489291 반응식
[CH2:1]([N:5]1[C:14](=[O:15])[C:13]([C:16]([OH:18])=O)=[C:12]2[C:7]([CH2:8][CH2:9][CH2:10][CH2:11]2)=[CH:6]1)[CH2:2][CH2:3][CH3:4].S(Cl)(Cl)=O.[CH2:23]([NH2:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.Cl>C1(C)C=CC=CC=1.C(Cl)Cl.CN(C=O)C>[CH2:23]([NH:30][C:16]([C:13]1[C:14](=[O:15])[N:5]([CH2:1][CH2:2][CH2:3][CH3:4])[CH:6]=[C:7]2[C:12]=1[CH2:11][CH2:10][CH2:9][CH2:8]2)=[O:18])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 7504BenzylamineHCID 24386Thionyl ChlorideHCID 222665212-Butyl-3-oxo-2,3,5,6,7,8-hexahydroisoquinoline-4-carboxylic acid

생성물 1

HCID 235880372-Butyl-3-oxo-2,3,5,6,7,8-hexahydroisoquinoline-4-carboxylic acid benzylamide수율 74%

시약·촉매·용매 3

HCID 1140
Toluene
용매
HCID 6228Dimethylformamide용매
HCID 6344Dichloromethane용매

실험 절차

2-Butyl-3-oxo-2,3,5,6,7,8-hexahydroisoquinoline-4-carboxylic acid (4-501-05) (5 mg, 0.02 mmol) was dissolved in toluene (1 mL), and to the reaction mixture were added thionyl chloride (4.4 μL, 0.06 mmol) and catalytic amount of DMF, and the reaction mixture was reacted at 75° C. for 30 min. After concentration of the reaction mixture under reduced pressure, the residue was dissolved in methylene chloride (1 mL), and then benzylamine (6.2 μL, 0.06 mmol) was added to the reaction mixture, and the reaction mixture was stirred at room temperature for 10 min. To the reaction mixture was added diluted hydrochloric acid (1 mol/L, 3 mL), and the reaction mixture was extracted with ethyl acetate (8 mL), washed with brine (4 mL), dried over anhydrous magnesium sulfate, and evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (toluene/ethyl acetate) to give 2-butyl-3-oxo-2,3,5,6,7,8-hexahydroisoquinoline-4-carboxylic acid benzylamide (4-501) (5 mg, 74%) as a white crystal.

후처리

  1. customthe reaction mixture was reacted at 75° C. for 30 min
  2. extractionthe reaction mixture was extracted with ethyl acetate (8 mL)
  3. washwashed with brine (4 mL)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography (toluene/ethyl acetate)

출처 및 근거

ORD 기록
ord-5f5726cebfe44ec78bb6f812d9093ec8
출처 데이터셋
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06977266B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트