Hydrochloric Acid → HCID 53661213、化合物

HRID 1168105

反応式

HRID 1168105 の反応式
[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]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 72886L-Cysteic acid2 回HCID 20205723n-BuOH HOAc EtOAc H2O

生成物 1

HCID 53661213HCID 53661213、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-750f38af12394e77b29ace4bf3b9e3ab
出典データセット
uspto-grants-2003_09
特許番号
US06623655B1

関連ノート

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