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Water → (3R,4R)-3-(2-hydroxyethyl)-4-[3-(R,S)-hydroxy-3-(6-methoxyquinolin-4-yl)propyl]-1-(tert-butyloxycarbonyl)piperidine

HRID 2186385
ノート
印刷プレビュー

反応式

HRID 2186385 の反応式
[O:1]=[C:2]([C:20]1[C:29]2[C:24](=[CH:25][CH:26]=[C:27]([O:30][CH3:31])[CH:28]=2)[N:23]=[CH:22][CH:21]=1)[CH2:3][CH2:4][C@@H:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][C@@H:6]1[CH:18]=[CH2:19].O.B(O[O-])=[O:34].[Na+].[Cl-].[NH4+]>C1(C)C=CC=CC=1.O1CCCC1>[OH:34][CH2:19][CH2:18][C@@H:6]1[C@H:5]([CH2:4][CH2:3][CH:2]([OH:1])[C:20]2[C:29]3[C:24](=[CH:25][CH:26]=[C:27]([O:30][CH3:31])[CH:28]=3)[N:23]=[CH:22][CH:21]=2)[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7]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 962WaterHCID 25517Ammonium ChlorideHCID 517072Sodium PerborateHCID 69345707(3R,4R)-1-tert-butyloxycarbonyl-4-[3-(6-methoxyquinolin-4-yl)-3-oxopropyl]-3-vinylpiperidine

生成物 1

HCID 69353248(3R,4R)-3-(2-hydroxyethyl)-4-[3-(R,S)-hydroxy-3-(6-methoxyquinolin-4-yl)propyl]-1-(tert-butyloxycarbonyl)piperidine収率 36.3%

試薬・触媒・溶媒

2
HCID 1140Toluene溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
110 °C

実験手順

33.4 cm3 of triethylamineborane complex were added with stirring, at a temperature in the region of 20° C., to a solution of 52.6 g of (3R,4R)-4-[3-oxo-3-(6-methoxyquinolin-4-yl)propyl]-1-(tert-butyloxycarbonyl)-3-vinylpiperidine in 500 cm3 of toluene and then the mixture was heated for 18 hours at a temperature in the region of 110° C. After having concentrated the reaction mixture under reduced pressure (5 kPa) at a temperature in the region of 45° C., the residue obtained was taken up in 500 cm3 of tetrahydrofuran. The solution which resulted therefrom had approximately 63 cm3 of water added over 20 minutes and then 47.5 g of sodium perborate were added portionwise over approximately 1 hour. The mixture was stirred for 4 hours at a temperature in the region of 20° C. and then 300 cm3 of a saturated ammonium chloride solution were added. The organic solution was separated by settling, dried over magnesium sulfate, and concentrated under the same conditions as above. The residue obtained was purified by chromatography on a column of silica gel (particle size 20-45 μm; diameter 9 cm; silica volume 2500 cm3), elution was carried out first with a dichloromethane/methanol (97.5/2.5 by volume) mixture, and 1-liter fractions were collected. Fractions 1 to 17 were separated and then elution was carried out with a dichloromethane/methanol (95/5 by volume) mixture, 1-liter fractions were collected. Fractions 30 to 35 were combined and, finally, elution was carried out with a dichloromethane/methanol (90/10 by volume) mixture, 1-liter fractions were collected. Fractions 36 to 41 were combined, while the combination of fractions 30 to 41 was evaporated under reduced pressure (5 kPa) at a temperature in the region of 40° C. 20 g of (3R,4R)-3-(2-hydroxyethyl)-4-[3-(R,S)-hydroxy-3-(6-methoxyquinolin-4-yl)propyl]-1-(tert-butyloxycarbonyl)piperidine were obtained in the form of an oil.

後処理

  1. addition33.4 cm3 of triethylamineborane complex were added
  2. concentrationAfter having concentrated the reaction mixture under reduced pressure (5 kPa) at a temperature in the region of 45° C.
  3. customthe residue obtained
  4. customThe solution which resulted
  5. additionadded over 20 minutes
  6. customThe organic solution was separated
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated under the same conditions as above
  9. customThe residue obtained
  10. customwas purified by chromatography on a column of silica gel (particle size 20-45 μm; diameter 9 cm; silica volume 2500 cm3), elution
  11. customwere collected
  12. customFractions 1 to 17 were separated
  13. washelution
  14. customwere collected
  15. washfinally, elution
  16. customwere collected
  17. customwas evaporated under reduced pressure (5 kPa) at a temperature in the region of 40° C

出典と根拠

ORDレコード
ord-2ae68d0c3c974b53b3da66fb6fbc6dfb
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06403610B1

反応ノート

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