反応 #362830

ord-6c6cf981a47b4307bfcdb6d7c3a31605

反応方程式

CC(C)(C)OC(=O)N[C@@H](Cc1ccc(OCCCl)cc1)C(=O)O
(S)-N-tert-butoxycarbonyl-4-O-(2-chloroethyl)tyrosine
Cl.N[C@@H](Cc1ccc(OCCCl)cc1)C(=O)O
(S)-4-O-(2-chloroethyl)tyrosine hydrochloride
収率 77.6%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他are placed in a round-bottomed flask
  2. 2
    濃縮the mixture is concentrated to dryness under reduced pressure
  3. 3
    workup.STIRRINGthis solution is then stirred
  4. 4
    ろ過filtered
  5. 5
    洗浄The resulting solid is washed with 2 times 25 ml of ether
  6. 6
    その他dried under reduced pressure in order

実験手順

5 g of (S)-N-tert-butoxycarbonyl-4-O-(2-chloroethyl)tyrosine, dissolved in 50 ml of hydrochloric dioxane, are placed in a round-bottomed flask. After having been stirred for 28 h, the mixture is concentrated to dryness under reduced pressure. The resulting residue is taken up in 50 ml of ether and this solution is then stirred and filtered. The resulting solid is washed with 2 times 25 ml of ether and then dried under reduced pressure in order to yield 1.58 g of (S)-4-O-(2-chloroethyl)tyrosine hydrochloride in the form of a white solid which melts at 260° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06352839B1uspto-grants-2002_03