Hydrochloric Acid → N-benzyl-beta-benzyl-D-serinamide

HRID 534676

反応式

HRID 534676 の反応式
[CH2:1]([NH:8][C:9](=[O:28])[C@@H:10]([CH2:19][O:20]CC1C=CC=CC=1)[NH:11]C(OC(C)(C)C)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>ClCCl>[CH2:1]([NH:8][C:9](=[O:28])[C@@H:10]([CH:19]([CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[OH:20])[NH2:11])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 7216909N-benzyl-O-benzyl-N2-Boc-D-serinamide

生成物 1

HCID 86669435N-benzyl-beta-benzyl-D-serinamide収率 89.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of N-benzyl-O-benzyl-N2-Boc-D-serinamide (1 g) and dichloromethane (5 mL), aq.HCl (20%) (5 mL) was added. The solution was stirred for 2 hours at room temperature for completion of reaction. The solution was concentrated under vacuum to remove dichloromethane and subsequently water was added. The aqueous layer was basified to pH 8-10 with 5% sodium hydroxide. The aqueous layer was extracted with ethyl acetate and the combined organic layer was washed with brine solution. Organic layer was concentrated under vacuum to obtain an oily residue 0.33 g of N-benzyl-β-benzyl-D-serinamide.

後処理

  1. concentrationThe solution was concentrated under vacuum
  2. customto remove dichloromethane and subsequently water
  3. additionwas added
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. washthe combined organic layer was washed with brine solution
  6. concentrationOrganic layer was concentrated under vacuum

出典と根拠

ORDレコード
ord-b57a19902d65452bbd7bac77b1dc4171
出典データセット
uspto-grants-2014_10
特許番号
US08853439B2

関連ノート

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