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

Acetic Anhydride → 1-acetoxy-1-(6-benzyloxy-2-naphthyl)-2-[2-(N,N-dimethylamino)ethoxy]ethane hydrochloride

HRID 1198258
노트
인쇄 미리보기

반응식

HRID 1198258 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[CH:15]=[C:14]([CH:19]([OH:27])[CH2:20][O:21][CH2:22][CH2:23][N:24]([CH3:26])[CH3:25])[CH:13]=[CH:12]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:28](OC(=O)C)(=[O:30])[CH3:29].C(=O)([O-])[O-].[K+].[K+].[ClH:41].C(O)C>N1C=CC=CC=1.CC(C)=O.O.C(OCC)(=O)C>[ClH:41].[C:28]([O:27][CH:19]([C:14]1[CH:13]=[CH:12][C:11]2[C:16](=[CH:17][CH:18]=[C:9]([O:8][CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH:10]=2)[CH:15]=1)[CH2:20][O:21][CH2:22][CH2:23][N:24]([CH3:25])[CH3:26])(=[O:30])[CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 21887872Ethanol hydrochlorideHCID 544081981-(6-benzyloxy-2-naphthyl)-2-[2-(N,N-dimethylamino)ethoxy]ethanol

생성물 1

HCID 675979821-acetoxy-1-(6-benzyloxy-2-naphthyl)-2-[2-(N,N-dimethylamino)ethoxy]ethane hydrochloride

시약·촉매·용매 4

HCID 180
Acetone
용매
HCID 962Water용매
HCID 1049Pyridine용매
HCID 8857Ethyl Acetate용매

실험 절차

In 12 ml of pyridine was suspended 3.0 g of 1-(6-benzyloxy-2-naphthyl)-2-[2-(N,N-dimethylamino)ethoxy]ethanol. To the suspension was added 1.6 ml of acetic anhydride. The resulting mixture was stirred at room temperature for 24 hours. After the completion of the reaction, the solvent was removed by distillation under reduced pressure. To the residue thus obtained were added 60 ml of ethyl acetate and 60 ml of water. The mixture was adjusted to pH 10.5 with potassium carbonate. The organic layer was separated. The aqueous layer was extracted with 30 ml of ethyl acetate. The extract was combined with the previously separated organic layer. The combined organiclayer was washed with water and a saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue thus obtained was dissolved in 30 ml of acetone. To the solution was added 1.5 ml of a 5N dry hydrogen chloride-ethanol solution. The resulting mixture was stirred at room temperature for 1 hour. The resulting cyrstals were collected by filtration and dried to obtain 2.6 g of 1-acetoxy-1-(6-benzyloxy-2-naphthyl)-2-[2-(N,N-dimethylamino)ethoxy]ethane hydrochloride (compound No. 286).

후처리

  1. customAfter the completion of the reaction
  2. customthe solvent was removed by distillation under reduced pressure
  3. customTo the residue thus obtained
  4. customThe organic layer was separated
  5. extractionThe aqueous layer was extracted with 30 ml of ethyl acetate
  6. washThe combined organiclayer was washed with water
  7. dry with materiala saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate
  8. customThe solvent was removed by distillation under reduced pressure
  9. customThe residue thus obtained
  10. stirringThe resulting mixture was stirred at room temperature for 1 hour
  11. filtrationThe resulting cyrstals were collected by filtration
  12. customdried

출처 및 근거

ORD 기록
ord-e45a3b36e5854a388ab462c64d4b72ac
출처 데이터셋
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05280032

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트