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Hydrochloric Acid → HCID 57539222, 화합물

HRID 601975
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HRID 601975 반응식
[NH2:1][C@H:2]([CH2:6][O:7][CH:8]([F:10])[F:9])[C:3]([OH:5])=[O:4].C(=O)(O)[O-].[Na+].[C:16](OC(=O)C)(=[O:18])[CH3:17].Cl>O.O1CCOCC1>[C:16]([NH:1][C@H:2]([CH2:6][O:7][CH:8]([F:10])[F:9])[C:3]([OH:5])=[O:4])(=[O:18])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 57539232HCID 57539232, 화합물

생성물 1

HCID 57539222HCID 57539222, 화합물수율 82.3%

시약·촉매·용매 2

HCID 962Water용매
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
HCID 31275
1,4-Dioxane
용매

실험 절차

(2R)-2-Amino-3-(difluoromethoxy)propanoic acid (680 mg, 4.39 mmol) was mixed with sodium bicarbonate (738 mg. 8.78 mmol) and acetic anhydride (491 mg, 4.82 mmol) in water (10 mL) and dioxane (10 mL) at 0° C. to room temperature overnight. The reaction mixture was acidified with 1N HCl to pH2, concentrated and extracted with ethyl acetate, and concentrated again to give (2R)-2-(Acetylamino)-3-(difluoromethoxy)propanoic acid (580 mg, 82.3%) as a colorless sticky oil. 1H NMR (300 MHz, CDCl3): δ(ppm) 6.40 (d, 1H), 6.24 (wt, 1H), 4.88 (m, 1H), 4.36 (dd, 1H), 4.22 (dd, 1H), 2.12 (s, 3H).

후처리

  1. concentrationconcentrated
  2. extractionextracted with ethyl acetate
  3. concentrationconcentrated again

출처 및 근거

ORD 기록
ord-ce40988c363a482e98ab0ffe7b4b441b
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07902401B2

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