Water → HCID 68972961, 화합물

HRID 1272687노트

반응식

HRID 1272687 반응식
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

참가 물질

6

반응물 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

생성물 1

HCID 68972961HCID 68972961, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ce8a7c21637043199a953561f5eefdba
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07208601B2

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