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Acetic Acid → ethyl (3S,4S)-4-{[(benzyloxy)carbonyl]amino}-3-hydroxy-5-methylhexanoate

HRID 2046656
ノート
印刷プレビュー

反応式

HRID 2046656 の反応式
C(N[CH:5]([CH3:7])[CH3:6])(C)C.C([Li])CCC.[C:13]([O:16][CH2:17][CH3:18])(=[O:15])[CH3:14].[CH:19]([C@@H:21]([NH:25][C:26](=[O:35])[O:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[CH:22]([CH3:24])[CH3:23])=[O:20].[C:36]([OH:39])(=[O:38])[CH3:37]>O1CCCC1.CCCCCC.O>[CH2:28]([O:27][C:26]([NH:25][C@@H:21]([CH:22]([CH3:24])[CH3:23])[C@@H:19]([OH:20])[CH2:14][C:13]([O:16][CH2:17][CH3:18])=[O:15])=[O:35])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.[CH2:28]([O:27][C:26]([NH:25][CH:37]([CH:13]([OH:15])[CH2:14][CH:5]([CH3:6])[CH3:7])[C:36]([O-:39])=[O:38])=[O:35])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=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

10

反応物 5

HCID 176Acetic AcidHCID 7912DiisopropylamineHCID 8857Ethyl AcetateHCID 11009915benzyl [(1S)-1-formyl-2-methylpropyl]carbamateHCID 178418339Butyllithium

生成物 2

HCID 59370506ethyl (3S,4S)-4-{[(benzyloxy)carbonyl]amino}-3-hydroxy-5-methylhexanoate
HCID 131731055
([(Benzyloxy)carbonyl]amino}-3-hydroxy-5-methylhexanoate

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒3 回HCID 8058Hexane溶媒

反応条件

温度
-78 °C

実験手順

To a solution (40 mL) of diisopropylamine (4.6 mL) in tetrahydrofuran was added 1.6 mol/L solution (20.19 mL) of n-butyllithium in hexane, and the mixture was cooled to −78° C. A solution (5 mL) of ethyl acetate (3.16 mL) in tetrahydrofuran was added dropwise to the mixture at a rate to maintain the reaction mixture at −70° C. or below. After the completion of the dropwise addition, the mixture was stirred at −78° C. for 1 hr, a solution (10 mL) of benzyl [(1S)-1-formyl-2-methylpropyl]carbamate (1.9 g) in tetrahydrofuran was added dropwise thereto at a rate to maintain the reaction mixture at −70° C. or below. The reaction mixture was once warmed to −30° C., and cooled again to −78° C. Acetic acid (2.3 mL) was added to the mixture, and the temperature of the mixture was raised to room temperature. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=9:1→2:1) to give the title compound (yield: 800 mg) and ethyl (3R,4S)-4-{([(benzyloxy)carbonyl]amino}-3-hydroxy-5-methylhexanoate (yield: 550 mg) both as a colorless oil.

後処理

  1. temperatureto maintain the reaction mixture at −70° C. or below
  2. additionAfter the completion of the dropwise addition
  3. temperatureat a rate to maintain the reaction mixture at −70° C. or below
  4. temperatureThe reaction mixture was once warmed to −30° C.
  5. temperaturecooled again to −78° C
  6. temperaturethe temperature of the mixture was raised to room temperature
  7. extractionthe mixture was extracted with ethyl acetate
  8. washThe extract was washed with saturated brine
  9. dry with materialdried over anhydrous sodium sulfate
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=9:1→2:1)

出典と根拠

ORDレコード
ord-972484da68c24c768cbd3f837d393ee4
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08592452B2

反応ノート

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