Hydrochloric Acid → HCID 18924114, 화합물

HRID 1291905노트

반응식

HRID 1291905 반응식
[CH3:1][N:2]([CH3:28])[C:3]1[CH:8]=[CH:7][N:6]=[CH:5][C:4]=1[CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:27]=[CH:26][C:16]([O:17][CH2:18][CH2:19][CH2:20][C:21]([O:23]CC)=[O:22])=[CH:15][CH:14]=1.[OH-].[Na+].Cl>CO>[CH3:28][N:2]([CH3:1])[C:3]1[CH:8]=[CH:7][N:6]=[CH:5][C:4]=1[CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[CH:15][C:16]([O:17][CH2:18][CH2:19][CH2:20][C:21]([OH:23])=[O:22])=[CH:26][CH:27]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 18918492HCID 18918492, 화합물

생성물 1

HCID 18924114HCID 18924114, 화합물수율 60.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of ethyl 4-[4-[3-(4-dimethylaminopyrid-3-yl)propyloxy]phenoxy]butyrate (160 mg) in methanol (10 ml) was added sodium hydroxide solution (2.0 ml of 1.0M) and the solution left until all starting ester had disappeared (Tlc). The reaction mixture was neutralised with hydrochloric acid (2.0 ml of 1.0 M) and evaporated in vacuo. A small amount (5 ml) of water was added and the resulting solution extracted with dichloromethane (3×15 ml). The organic extracts were combined, dried (PS paper) and evaporated to yield the title compound as colourless prisms, (90 mg) m.p. 106°-108° C. (from ethyl acetate); NMR (d6DMSO) : δ 1.8-2.1 (2H,q;2H,q); 2.4 (2H,t); 2.8 (2H,t;6H,s); 3.9 (2H,t;2H,t); 6.8(5H,m); 8.2 (2H,d); m/e 359 (M+H)+ ; calculated for C20 H26N2O4 : C,67.0; H,7.3; N,7.8; found : C,67.1; H,7.6;N,7.7%.

후처리

  1. customevaporated in vacuo
  2. additionA small amount (5 ml) of water was added
  3. extractionthe resulting solution extracted with dichloromethane (3×15 ml)
  4. customdried (PS paper)
  5. customevaporated

출처 및 근거

ORD 기록
ord-e97e43308c334b049a6b4deb3ddb5e01
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753659

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