Hydrochloric Acid → HCID 57673909, 화합물

HRID 490058노트

반응식

HRID 490058 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 57673909HCID 57673909, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3686e9d92cd049048910744240f2e15e
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07528120B2

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