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Sodium Carbonate → HCID 53706240、化合物

HRID 276717
ノート
印刷プレビュー

反応式

HRID 276717 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][CH:13]=1)[CH2:5][C@@H:6]([C:8]([OH:10])=[O:9])[NH2:7].C([O-])([O-])=O.[Na+].[Na+].[C:20]1([CH:26]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:27](Cl)=[O:28])[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>O.C1COCC1>[CH3:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][CH:13]=1)[CH2:5][C@@H:6]([C:8]([OH:10])=[O:9])[NH:7][C:27](=[O:28])[CH:26]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=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 10340Sodium CarbonateHCID 746372,2-Diphenylacetyl chlorideHCID 27614943-Methylphenylalanine

生成物 1

HCID 53706240HCID 53706240、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 3-methyl-L-phenylalanine (1.8 g, 10.06 mmol) and Na2CO3 (3.2 g, 3.0.18 mmol) in water (150 mL) is added a solution of diphenylacetyl chloride (2.32 g, 10.06 mmol) in THF (150 mL), and the resulting solution is stirred vigorously at room temperature overnight. The THF is then evaporated and the aqueous layer is diluted with 6% aqueous Na2CO3 (100 mL), and washed with Et2O (3×150 mL). The aqueous layer is then acidified to pH 1 with conc. HCl, and the resulting slurry is extracted with EtOAc (3×100 mL). The organic phase is then washed with water (2×100 mL) and brine (1×100 mL), dried over MgSO4 and evaporated to yield 3-methyl-N-(2,2-diphenylacetyl)-L-phenylalanine, as a white solid.

後処理

  1. customThe THF is then evaporated
  2. additionthe aqueous layer is diluted with 6% aqueous Na2CO3 (100 mL)
  3. washwashed with Et2O (3×150 mL)
  4. extractionthe resulting slurry is extracted with EtOAc (3×100 mL)
  5. washThe organic phase is then washed with water (2×100 mL) and brine (1×100 mL)
  6. dry with materialdried over MgSO4
  7. customevaporated

出典と根拠

ORDレコード
ord-60f8bb385ef446c28b2977ed12a20ca8
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06353017B1

反応ノート

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