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N-Hydroxyphthalimide → HCID 59479004, 화합물

HRID 450750
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HRID 450750 반응식
[OH:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([NH2:9])=[O:8])=[CH:5][N:4]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O[N:32]1[C:36](=[O:37])[C:35]2=[CH:38][CH:39]=[CH:40][CH:41]=[C:34]2[C:33]1=[O:42].N(C(OC(C)C)=O)=NC(OC(C)C)=O>O.C(OCC)(=O)C.C1COCC1>[O:42]=[C:33]1[C:34]2[C:35](=[CH:38][CH:39]=[CH:40][CH:41]=2)[C:36](=[O:37])[N:32]1[O:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([NH2:9])=[O:8])=[CH:5][N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 10665N-HydroxyphthalimideHCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 450843336-(Hydroxymethyl)nicotinamide

생성물 1

HCID 59479004HCID 59479004, 화합물수율 47.7%

시약·촉매·용매 3

HCID 962Water
용매
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of 313 mg of 6-(hydroxymethyl)nicotinamide, 540 mg of triphenylphosphine, 503 mg of N-hydroxyphthalimide, and 4.7 ml of THF was added dropwise 0.53 ml of diisopropyl azodicarboxylate, followed by stirring overnight. After concentration, the solid thus produced was suspended in water, and ethyl acetate was added thereto. After stirring for 30 minutes, the solid was collected by filtration to obtain 292 mg of 6-{[(1,3-dioxo-1,3-dihydro-2H-isoindo1-2-yl)oxy]methyl}nicotinamide.

후처리

  1. concentrationAfter concentration
  2. customthe solid thus produced
  3. stirringAfter stirring for 30 minutes
  4. filtrationthe solid was collected by filtration

출처 및 근거

ORD 기록
ord-48ecb43fee3442588cdae7b0ac209325
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486970B2

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