Water → HCID 68972961、化合物

HRID 1272687ノート

反応式

HRID 1272687 の反応式
Cl.[CH3:2][O:3][C:4](=[O:14])[C@H:5]([NH2:13])[CH2:6][C:7]1[S:8][C:9]([Br:12])=[CH:10][CH:11]=1.N[C@H](CC1S[C:23](Br)=[CH:24][CH:25]=1)C(O)=O.[C:27]([O-:30])(O)=[O:28].[Na+].O.[CH2:33](Cl)Cl>>[CH3:2][O:3][C:4](=[O:14])[C@H:5]([NH:13][C:27]([O:30][C:24]([CH3:23])([CH3:25])[CH3:33])=[O:28])[CH2:6][C:7]1[S:8][C:9]([Br:12])=[CH:10][CH:11]=1

参加物

6

反応物 5

HCID 962WaterHCID 6344DichloromethaneHCID 516892Sodium BicarbonateHCID 7016818(R)-2-Amino-3-(5-bromothiophen-2-yl)propanoic acidHCID 68974038(2R)-amino-3-(5-bromo-thiophen-2-yl)-propionic acid methyl ester HCl

生成物 1

HCID 68972961HCID 68972961、化合物

実験手順

To a suspension of (2R)-amino-3-(5-bromo-thiophen-2-yl)-propionic acid methyl ester HCl (14.0 g, 46.59 mmol) (prepared from commercially available (2R)-amino-3-(5-bromo-thiophen-2-yl)-propionic acid) in DCM (250 mL) was added NaHCO3 (9.78 g, 116.49 mmol), water (100 mL). The solution was stirred for 10 min and Boc-anhydride (12.20 g, 55.91 mmol) was added. The reaction was stirred overnight. The organic layer was separated and washed with brine, dried (Na2SO4) and concentrated under reduced pressure to give 17.0 g of 3-(5-bromo-thiophen-2-yl)-2(R)-tert-butoxycarbonylamino-propionic acid methyl ester.

後処理

  1. stirringThe reaction was stirred overnight
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-ce8a7c21637043199a953561f5eefdba
出典データセット
uspto-grants-2007_04
特許番号
US07208601B2

反応ノート

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