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

Benzaldehyde → HCID 70527317, 화합물

HRID 2057397
노트
인쇄 미리보기

반응식

HRID 2057397 반응식
C[C:2]([CH2:12]C(O)C[OH:15])([CH3:11])[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[CH:17](=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=CC=1.[C:25]([OH:33])(=[O:32])[C:26]1C=CC=C[CH:27]=1.ClC1C=CC=[CH:37][N:36]=1.C[N:42]([CH:44]=[O:45])C>C1C=CC=CC=1>[C:44]([OH:45])(=[O:15])/[CH:27]=[CH:26]\[C:25]([OH:33])=[O:32].[CH3:12][C:2]([NH:36][CH2:37][CH:25]([OH:33])[CH2:26][O:24][C:17]1[CH:18]=[CH:23][CH:22]=[CH:21][N:42]=1)([CH3:11])[CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 240BenzaldehydeHCID 243Benzoic AcidHCID 6228DimethylformamideHCID 79772-ChloropyridineHCID 20534797HCID 20534797, 화합물

생성물 1

HCID 70527317HCID 70527317, 화합물

시약·촉매·용매 1

HCID 241
Benzene
용매

반응 조건

온도
70 °C

실험 절차

A solution of 3.9 g. (16 mmole) 3-(1,1-dimethyl-3-phenylpropyl)-1,2-dihydroxypropane, 15 ml. benzaldehyde, 9 ml. benzene, and 100 mg. benzoic acid was refluxed for 16 hours while a Dean=Stark trap was being used to collect the water. The solution was diluted with benzene and washed with aqueous potassium carbonate. The mixture was concentrated and the residue was distilled under reduced pressure (0.4 mm.) at a pot temperature of 75°-80° C. The residue from above in 50 ml. DMF was then added dropwise to sodium hydride (1.0 g. of a 50% oil dispersion washed with hexane) in 25 ml. DMF. After the addition, stirring was continued for 1 hour. 2-Chloropyridine (1.80 g., 16 mmole) in 25 ml. DMF was added and the mixture heated at 70° C. for 16 hours. Most of the DMF was evaporated. Water and ether were added and the layers separated. The ether solution was washed twice with 100 ml. 4N HCl and the combined acid washings were heated on a steam bath for 1/2 hour. After washing with ether, the aqueous phase was made basic with KOH. The oil was extracted with CH2Cl2, dried (Na2SO4), and concentrated to give 3.0 g. (60%) of the crude free base. A small sample was used to prepare the maleate salt in 2-propanol/ether, and recrystallization of this from 2-propanol gave pure 2-[3-(1,1-dimethyl-3-phenylpropylamino)-2-hydroxy-1-propoxy]pyridine maleate; mp 144°-146° C.

후처리

  1. customto collect the water
  2. additionThe solution was diluted with benzene
  3. washwashed with aqueous potassium carbonate
  4. concentrationThe mixture was concentrated
  5. distillationthe residue was distilled under reduced pressure (0.4 mm.) at a pot temperature of 75°-80° C
  6. additionDMF was then added dropwise to sodium hydride (1.0 g
  7. washof a 50% oil dispersion washed with hexane) in 25 ml
  8. additionAfter the addition
  9. customMost of the DMF was evaporated
  10. additionWater and ether were added
  11. customthe layers separated
  12. washThe ether solution was washed twice with 100 ml
  13. temperature4N HCl and the combined acid washings were heated on a steam bath for 1/2 hour
  14. washAfter washing with ether
  15. extractionThe oil was extracted with CH2Cl2
  16. dry with materialdried (Na2SO4)
  17. concentrationconcentrated
  18. customto give 3.0 g
  19. customto prepare
  20. customthe maleate salt in 2-propanol/ether, and recrystallization of this from 2-propanol

출처 및 근거

ORD 기록
ord-227ac86bb43b4234983984c6e4c432f8
출처 데이터셋
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04210653

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트