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Benzyl chloroformate → rac-Methyl-2-{[(benzyloxy)carbonyl]amino}-6,6,7,7,7-pentafluoroheptanoate

HRID 1844198
ノート
印刷プレビュー

反応式

HRID 1844198 の反応式
Cl.[CH3:2][O:3][C:4](=[O:17])[CH:5]([NH2:16])[CH2:6][CH2:7][CH2:8][C:9]([F:15])([F:14])[C:10]([F:13])([F:12])[F:11].C(=O)([O-])[O-].[K+].[K+].[C:24](Cl)(=[O:33])[O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1>C1COCC1.O>[CH3:2][O:3][C:4](=[O:17])[CH:5]([NH:16][C:24]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[O:33])[CH2:6][CH2:7][CH2:8][C:9]([F:14])([F:15])[C:10]([F:11])([F:12])[F:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10387Benzyl chloroformateHCID 11430Potassium CarbonateHCID 90115377Rac-methyl-2-amino-6,6,7,7,7-pentafluoroheptanoate hydrochloride

生成物 1

HCID 90115438rac-Methyl-2-{[(benzyloxy)carbonyl]amino}-6,6,7,7,7-pentafluoroheptanoate

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

Under argon, 16.9 g (59.2 mmol) of rac-methyl-2-amino-6,6,7,7,7-pentafluoroheptanoate hydrochloride (racemate) from Example 139A were initially charged in 775 ml of THF and 99 ml of water, and 25.37 g (183.6 mmol) of potassium carbonate were added carefully at RT. 11.0 ml (65.1 mmol) of benzyl chlorocarbonate were then added dropwise at 0° C., and the suspension was stirred at RT overnight. The reaction mixture was concentrated, water was added to the residue and the mixture was extracted twice with dichloromethane. The combined organic phases were dried over sodium sulphate, filtered and concentrated. The crude product was purified by silica gel chromatography (mobile phase: cyclohexane/ethyl acetate gradient: 100/0 to 10/1 to 8/1 to 5/1). The product fraction was then re-purified by preparative RP-HPLC (acetonitrile/water gradient with 0.1% TFA). This gave 13.34 g (56% of theory, purity 94%) of the target compound.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additionwater was added to the residue
  3. extractionthe mixture was extracted twice with dichloromethane
  4. dry with materialThe combined organic phases were dried over sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude product was purified by silica gel chromatography (mobile phase: cyclohexane/ethyl acetate gradient: 100/0 to 10/1 to 8/1 to 5/1)
  8. customThe product fraction was then re-purified by preparative RP-HPLC (acetonitrile/water gradient with 0.1% TFA)

出典と根拠

ORDレコード
ord-eabc0ccc8bdc43fab3d36f0b283b511f
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946215B2

反応ノート

読み込み中…

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