Triphenylphosphine → HCID 59348026, 화합물

HRID 2038637

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HRID 2038637 반응식
[OH:1][CH2:2][C:3]([CH3:9])([CH3:8])[C:4]([O:6][CH3:7])=[O:5].O[C:11]1[CH:21]=[CH:20][CH:19]=[C:13]2[C:14]([NH:16][C:17](=[O:18])[C:12]=12)=[O:15].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>O1CCCC1>[CH3:7][O:6][C:4](=[O:5])[C:3]([CH3:9])([CH3:8])[CH2:2][O:1][N:16]1[C:17](=[O:18])[C:12]2[C:13](=[CH:19][CH:20]=[CH:21][CH:11]=2)[C:14]1=[O:15]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 84152Methyl 3-hydroxypivalateHCID 3460024-hydroxy-2,3-dihydro-1H-isoindole-1,3-dione

생성물 1

HCID 59348026HCID 59348026, 화합물수율 33.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To methyl hydroxypivalate (1.31 g, 9.89 mmol) were added tetrahydrofuran (40 ml), hydroxyphthalimide (3.23 g, 19.78 mmol) and triphenylphosphine (6.48 g, 24.73 mmol). After this solution was cooled to 0° C., diisopropyl azodicarboxylate (4.87 ml, 24.73 mmol) was added dropwise to the solution. While being allowed to warm gradually, the reaction mixture was stirred for 12 hours, and concentrated under reduced pressure. The residue was roughly purified by silica gel column chromatography to give the title compound (922 mg).

후처리

  1. temperatureto warm gradually
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was roughly purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-538ef0658ace4e0ab2550a2b7a8d5014
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08575391B2

연결된 노트

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