Benzene → 24-Hydroxyvitamin D2

HRID 1857067노트

반응식

HRID 1857067 반응식
[CH3:1][CH:2]([C@:4]([OH:30])(/[CH:6]=[CH:7]/[C@H:8]([C@@H:10]1[C@:27]2([CH3:28])[C@H:13]([C:14]3[C@H:24]([CH2:25][CH2:26]2)[C@:22]2([CH3:23])[C:17]([CH2:18][C@@H:19]([OH:29])[CH2:20][CH2:21]2)=[CH:16][CH:15]=3)[CH2:12][CH2:11]1)[CH3:9])[CH3:5])[CH3:3].C1C=CC=CC=1.O>CCOCC>[CH3:9][C@@H:8]([C@@H:10]1[C@@:27]2([CH3:28])[CH2:26][CH2:25][CH2:24]/[C:14](=[CH:15]\[CH:16]=[C:17]3\[CH2:18][C@@H:19]([OH:29])[CH2:20][CH2:21][C:22]\3=[CH2:23])/[C@@H:13]2[CH2:12][CH2:11]1)/[CH:7]=[CH:6]/[C:4]([OH:30])([CH:2]([CH3:1])[CH3:3])[CH3:5]

참가 물질

5

반응물 3

HCID 241BenzeneHCID 962WaterHCID 69330425HCID 69330425, 화합물

생성물 1

HCID 644381324-Hydroxyvitamin D2수율 55.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

One gram (2.4 mmol) of (7) was dissolved in 250 ml of ether and benzene (4:1) and irradiated with stirring under nitrogen in a water-cooled quartz immersion well using a Hanovia medium-pressure UV lamp for 2 hrs. The solution was concentrated in vacuo, redissolved in 100 ml of ethanol and heated under reflux overnight. The solution was concentrated to dryness in vacuo and the residue was purified on a silica gel column using 30% ethyl acetate in hexane to yield 0.55 g (55%) of (8).

후처리

  1. customfor 2 hrs
  2. concentrationThe solution was concentrated in vacuo
  3. dissolutionredissolved in 100 ml of ethanol
  4. temperatureheated
  5. temperatureunder reflux overnight
  6. concentrationThe solution was concentrated to dryness in vacuo
  7. customthe residue was purified on a silica gel column

출처 및 근거

ORD 기록
ord-2b2091626e3444718fc37fedcbabf9c3
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06143910

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