Phosphate → Calcitriol

HRID 2259556

반응식

HRID 2259556 반응식
CCN(C1C=CC2C3(C4C(OC=2C=1)=CC(C)=C(NC1C=CC=CC=1)C=4)OC(=[O:20])C1C3=CC=CC=1)CC.P([O-])([O-])([O-])=O.[CH3:42][C@@H:43]([C@@H:50]1[C@@:54]2([CH3:70])[CH2:55][CH2:56][CH2:57]/[C:58](=[CH:59]\[CH:60]=[C:61]3\[CH2:62][C@@H:63]([OH:69])[CH2:64][C@H:65]([OH:68])[C:66]\3=[CH2:67])/[C@@H:53]2[CH2:52][CH2:51]1)[CH2:44][CH2:45][CH2:46][CH:47]([CH3:49])[CH3:48].C(Cl)Cl>C(O)C>[CH3:42][C@@H:43]([C@@H:50]1[C@@:54]2([CH3:70])[CH2:55][CH2:56][CH2:57]/[C:58](=[CH:59]\[CH:60]=[C:61]3\[CH2:62][C@@H:63]([OH:69])[CH2:64][C@H:65]([OH:68])[C:66]\3=[CH2:67])/[C@@H:53]2[CH2:52][CH2:51]1)[CH2:44][CH2:45][CH2:46][C:47]([OH:20])([CH3:48])[CH3:49]

참가 물질

6

반응물 4

HCID 1061PhosphateHCID 6344DichloromethaneHCID 1224022-Anilino-3-methyl-6-diethylaminofluoranHCID 5282181Alfacalcidol

생성물 1

HCID 5280453Calcitriol

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Nocardia autotrophica N-102 in the same BG medium (100 ml/500 ml-Erlenmeyer flask) as used in Example 1 was cultured at 28° C. under the aerobic conditions for 48 hours. To the culture medium were added 10 ml of a 5% PMCD solution (0.01 M phosphate buffer, pH 7.0) and a solution of 0.1% 1α-hydroxyvitamin D3 in 1 ml of ethanol (in the amount of 140 mol of PMCD relative to 1 mol of 1α-hydroxytvitamin D3). After cultivation for a further 2 hours, methylene chloride was added to the flask, and analysis was carried out according to the method as described in Example 3. The peak fraction having a retention time of 12 minutes was collected, concentrated at 40° C. or below under reduced pressure and applied to HPLC on Zorbax ODS column (4.6 mm×25 cm, made by Du Pont Co., USA) with water-methanol (1:9) as a mobile phase at a flow rate of 1.0 ml/min. After elution, the peak fraction having a retention time of 5.6 minutes was collected and concentrated to dryness at 40° C. or below under reduced pressure with a nitrogen gas replacement to give 650 μg (65% of the conversion ratio from the material) of 1α,25-dihydroxyvitamin D3. On the other hand, following the same procedure as above but without PMCD, the amount of 25-hydroxyvitamin D3 obtained was 350 μg/ml (35% of the conversion ratio from the material).

후처리

  1. waitAfter cultivation for a further 2 hours
  2. customwas collected
  3. concentrationconcentrated at 40° C. or below under reduced pressure
  4. washAfter elution
  5. customwas collected
  6. concentrationconcentrated to dryness at 40° C. or below under reduced pressure with a nitrogen gas replacement

출처 및 근거

ORD 기록
ord-c7eeb1c86c4a4456b2619197351e367d
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05474923

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