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Ammonium Chloride → Ethyl 4-benzyloxycarbonylamino-2,2-difluoro-3-hydroxy-5-phenylpentanoate

HRID 1859642
ノート
印刷プレビュー

反応式

HRID 1859642 の反応式
[CH2:1]([O:8][C:9]([NH:11][CH:12]([CH:20]=[O:21])[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[C:23]([F:30])([F:29])[C:24]([O:26][CH2:27][CH3:28])=[O:25].[Cl-].[NH4+]>[Zn].C1COCC1>[CH2:1]([O:8][C:9]([NH:11][CH:12]([CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[CH:20]([OH:21])[C:23]([F:30])([F:29])[C:24]([O:26][CH2:27][CH3:28])=[O:25])=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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 25517Ammonium Chloride2 回HCID 69585Ethyl bromodifluoroacetateHCID 11323549Benzyl (1-oxo-3-phenylpropan-2-yl)carbamate

生成物 1

HCID 10549370Ethyl 4-benzyloxycarbonylamino-2,2-difluoro-3-hydroxy-5-phenylpentanoate収率 91.3%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a mixture of the objective compound of step (10) (42.8 g, 0.151 mol), zinc dust (15.9 g, 0.243 mol) and THF (105 ml) was added ethyl bromodifluoroacetate (31.6 mL, 0.246 mol) with dropwise over 2 hours at 26˜49° C. The resulting mixture was stirred at room temperature for 2 hours. To this reaction mixture was added saturated ammonium chloride aqueous solution (110 mL), and the mixture was stirred for a few minutes. The obtained mixture was added to saturated ammonium chloride aqueous solution (650 mL) and extracted with ethyl acetate (500 mL, 2×300 mL). The extract was washed with saturated brine (400 mL), dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (2:1 hexane-ethyl acetate) to give 56.15 g of ethyl 4-benzyloxycarbonylamino-2,2-difluoro-3-hydroxy-5-phenylpentanoate as a light-yellow oil (a mixture of diastereomers, 75%).

後処理

  1. stirringthe mixture was stirred for a few minutes
  2. extractionextracted with ethyl acetate (500 mL, 2×300 mL)
  3. washThe extract was washed with saturated brine (400 mL)
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (2:1 hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-0bd87b20f67f4ce6a452470c93db8873
出典データセット
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06528514B1

反応ノート

読み込み中…

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