Hydrochloric Acid → HCID 53661213, 화합물

HRID 1168105

반응식

HRID 1168105 반응식
[NH2:1][C@H:2]([C:8]([OH:10])=[O:9])[CH2:3][S:4](=[O:7])([OH:6])=[O:5].Cl.[CH2:12](O)CCC.C(OCC)(=O)C.C(O)(=O)C.O>O1CCOCC1.CO>[CH3:12][O:9][C:8](=[O:10])[C@H:2]([CH2:3][S:4](=[O:6])([OH:7])=[O:5])[NH2:1]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 72886L-Cysteic acid2회HCID 20205723n-BuOH HOAc EtOAc H2O

생성물 1

HCID 53661213HCID 53661213, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

A mixture of 1 g of L-cysteic acid, 8 ml of 4 N hydrochloric acid in dioxane and 30 ml dry methanol was placed in a bottle. The bottle was capped and stored for approximately 96 hours at room temperature. Thin layer chromatography of the clear solution [Analtech silica gel plates, n-butanol:ethyl acetate:acetic acid:water (1:1:1:1), chlorine/potassium iodide-starch reagent (Stewart J. M. and Young J. D. in Solid Phase Peptide Synthesis, Pierce Chemical Company, PP.120 (1984)] indicated greater than 95 % conversion of cysteic acid to the ester. Solvents were removed under vacuum to get 1.05 g of a sticky solid. Mass spec analysis gave the m/z for the major M+1 ion as 184.3. Fragmentation of this ion gave the M+1 ion of 123.9, which represents the loss of one of the carboxymethyl groups. The solids were used without further purification in the next step.

후처리

  1. customThe bottle was capped
  2. customSolvents were removed under vacuum

출처 및 근거

ORD 기록
ord-750f38af12394e77b29ace4bf3b9e3ab
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06623655B1

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