Hydrochloric Acid → HCID 57673909、化合物

HRID 490058ノート

反応式

HRID 490058 の反応式
[NH2:1][C:2]([CH2:25][OH:26])([CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:13][CH:12]=1)[CH2:3][O:4][P:5](=[O:8])([OH:7])[OH:6].C(N([CH2:43][C:44]([OH:46])=O)CC(O)=O)CN(CC(O)=O)CC(O)=O.B(O)(O)O.Cl>C(O)C>[OH:26][CH2:25][C:2]([N:1]1[CH2:12][C:11]2[C:43](=[CH:3][CH:2]=[CH:9][CH:10]=2)[C:44]1=[O:46])([CH2:9][CH2:10][C:11]1[CH:12]=[CH:13][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:15][CH:16]=1)[CH2:3][O:4][P:5](=[O:6])([OH:7])[OH:8]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6049Ethylenediaminetetraacetic AcidHCID 7628Boric AcidHCID 9908268Fingolimod phosphate

生成物 1

HCID 57673909HCID 57673909、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The endproduct of step d) ((R/S)-FTY720-phosphate) (50 mg; 0.125 mmol) is suspended in a solution of EDTA (0.5 ml; 10 mM in water) and aqueous boric acid (0.5 ml; 3% in water; adjusted to pH 10.5 with aqueous KOH10%). After addition of OPA (33 mg, 0.25 mmol), dissolved in ethanol (0.5 ml), the reaction is kept at RT for 1 hour (ultrasound). After that the pH is adjusted to 3.5 (aqueous HCl; 1N) and extracted with ethylacetate (three times). The organic layer is dried over Na2SO4 and the compound is purified on silica gel using methylenechloride/methanol (95/5→0/100) as mobile phase.

後処理

  1. additionAfter addition of OPA (33 mg, 0.25 mmol)
  2. extractionextracted with ethylacetate (three times)
  3. dry with materialThe organic layer is dried over Na2SO4
  4. customthe compound is purified on silica gel

出典と根拠

ORDレコード
ord-3686e9d92cd049048910744240f2e15e
出典データセット
uspto-grants-2009_05
特許番号
US07528120B2

反応ノート

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