Triphenylphosphine → HCID 67229299, 화합물

HRID 600773

반응식

HRID 600773 반응식
[CH2:1]([O:3][C:4]1[CH2:5][C:6]2[C:11]([CH2:12][CH:13]=1)=[CH:10][CH:9]=[CH:8][C:7]=2[N:14]=[C:15]=S)[CH3:2].[N:17]([CH2:20][C:21]([C:23]1[CH:28]=[CH:27][C:26]([C:29]([F:32])([F:31])[F:30])=[CH:25][CH:24]=1)=[O:22])=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCOCC1>[CH2:1]([O:3][C:4]1[CH2:5][C:6]2[C:7]([NH:14][C:15]3[O:22][C:21]([C:23]4[CH:28]=[CH:27][C:26]([C:29]([F:30])([F:31])[F:32])=[CH:25][CH:24]=4)=[CH:20][N:17]=3)=[CH:8][CH:9]=[CH:10][C:11]=2[CH2:12][CH:13]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 11776TriphenylphosphineHCID 53416493HCID 53416493, 화합물HCID 866096122-Ethoxy-8-isothiocyanato-1,4-dihydronaphthalene

생성물 1

HCID 67229299HCID 67229299, 화합물수율 22%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of the product of Example 1F (398 mg, 1.72 mmol), the product of Example 1G (473 mg, 2.07 mmol), and triphenyl phosphine (542 mg, 2.07 mmol) in dioxane (9 mL) was heated at 85° C. for 30 min. The solution was cooled to room temperature and evaporated in vacuo. The residue was chromatographed on silica gel, eluting with 25% ethyl acetate-hexane to afford the title compound as a yellow solid (150 mg, 22%). 1H NMR (DMSO-d6) δ 9.38 (s, 1H), 7.76 (m, 4H), 7.65 (d, 1H, J=8.5 Hz), 7.62 (s, 1H), 7.18 (t, 1H, J=8.2 Hz), 6.97 (d, 1H, J=8.4 Hz), 4.85 (m, 1H), 3.79 (q, 2H, J=6.7 Hz), 3.49 (m, 2H), 3.36 (m, 2H), 1.26 (t, 3H, J=6.8 Hz); MS (ESI+) m/z 401 (M+H)+.

후처리

  1. customevaporated in vacuo
  2. customThe residue was chromatographed on silica gel
  3. washeluting with 25% ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-b41cf446029949bbb8ffd8e5c20401fe
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902236B2

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