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N-Hydroxyphthalimide → HCID 11388071, 화합물

HRID 620751
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HRID 620751 반응식
[CH:1]([O:14][N:15]1[CH:20]=[C:19]([O:21][CH:22]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:18](=[O:35])[CH:17]=[C:16]1[CH2:36][OH:37])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O[N:39]1[C:43](=[O:44])[C:42]2=[CH:45][CH:46]=[CH:47][CH:48]=[C:41]2[C:40]1=[O:49].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[N+](C(OCC)=O)(C(OCC)=O)=[N-]>CN(C)C=O.O.C(OCC)(=O)C.O1CCCC1>[C:43]1(=[O:44])[N:39]([O:37][CH2:36][C:16]2[N:15]([O:14][CH:1]([C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH:20]=[C:19]([O:21][CH:22]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[C:18](=[O:35])[CH:17]=2)[C:40](=[O:49])[C:41]2=[CH:48][CH:47]=[CH:46][CH:45]=[C:42]12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 10665N-HydroxyphthalimideHCID 11776TriphenylphosphineHCID 117521734(1H)-Pyridinone, 1,5-bis(diphenylmethoxy)-2-(hydroxymethyl)-HCID 14357405Diethyldiazodicarboxylate

생성물 1

HCID 11388071HCID 11388071, 화합물수율 50.2%

시약·촉매·용매 4

HCID 962
Water
용매
HCID 6228Dimethylformamide용매
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

실험 절차

12.3 g (0.0251 mol) of the product of Step (3) was added and dissolved in dimethylformamide (125 ml). Then, dried tetrahydrofuran (250 ml), 4.1 g (0.0251 mol) of N-hydroxyphthalimide and 9.9 g (0.0376 mol) of triphenylphosphine were added thereto. Further, 5.8 ml (0.0377 mol) of diethyl diazodicarboxylate was dropwise added under cooling with ice. The mixture was stirred at the same temperature for 10 minutes, and then ethyl acetate (500 ml) and water (1,500 ml) were added thereto. The ethyl acetate layer was washed with water and a saturated sodium chloride solution, and then dried over anhydrous magnesium sulfate, and then concentrated to dryness. The residue was subjected to silica gel column chromatography and eluted by benzene/ethyl acetate (4/1) to obtain 8.0 g of the above identified compound (yield: 50.2%)

후처리

  1. temperatureunder cooling with ice
  2. washThe ethyl acetate layer was washed with water
  3. dry with materiala saturated sodium chloride solution, and then dried over anhydrous magnesium sulfate
  4. concentrationconcentrated to dryness
  5. washeluted by benzene/ethyl acetate (4/1)
  6. customto obtain 8.0 g of the

출처 및 근거

ORD 기록
ord-9f73394bd9ec480eb777868bcbd73f06
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04822786

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