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Benzaldehyde → HCID 70527317、化合物

HRID 2057398
ノート
印刷プレビュー

反応式

HRID 2057398 の反応式
[CH3:1][C:2]([NH:12][CH2:13][CH:14]([OH:17])[CH2:15][OH:16])([CH3:11])[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.C(=[O:25])C1C=CC=CC=1.[C:26]([OH:34])(=[O:33])C1C=CC=CC=1.Cl[C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][N:37]=1>CN(C=O)C.C1C=CC=CC=1>[C:15]([OH:16])(=[O:25])/[CH:14]=[CH:13]\[C:26]([OH:34])=[O:33].[CH3:11][C:2]([NH:12][CH2:13][CH:14]([OH:17])[CH2:15][O:16][C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][N:37]=1)([CH3:1])[CH2:3][CH2:4][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 240BenzaldehydeHCID 243Benzoic AcidHCID 79772-ChloropyridineHCID 12855751HCID 12855751、化合物

生成物 1

HCID 70527317HCID 70527317、化合物

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 6228
Dimethylformamide
溶媒

反応条件

温度
70 °C

実験手順

A solution of 3.9 g. (16 mmole) 3-(1,1-dimethyl-3-phenylpropylamino)-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.

後処理

  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. additionThe residue from above in 50 ml DMF 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. customdried (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

出典と根拠

ORDレコード
ord-213a578a111f4853bcefdfc399223860
出典データセット
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04210653

反応ノート

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