Triphenylphosphine → HCID 140352849, 화합물

HRID 1194945노트

반응식

HRID 1194945 반응식
[CH2:1]=[C:2]1[CH2:7][CH2:6][CH:5]([OH:8])[CH2:4][CH2:3]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O/[N:29]=[C:30](/[C:36]1[N:37]=[C:38]([NH:41][C:42]([C:55]2[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=2)([C:49]2[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=2)[C:43]2[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=2)[S:39][CH:40]=1)\[C:31]([O:33][CH2:34][CH3:35])=[O:32].N(C(OC)=O)=NC(OC)=O>C1C=CC=CC=1>[CH2:1]=[C:2]1[CH2:7][CH2:6][CH:5]([O:8]/[N:29]=[C:30](/[C:36]2[N:37]=[C:38]([NH:41][C:42]([C:55]3[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=3)([C:49]3[CH:50]=[CH:51][CH:52]=[CH:53][CH:54]=3)[C:43]3[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=3)[S:39][CH:40]=2)\[C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH2:4][CH2:3]1

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 351621Azodicarboxylic acid dimethyl esterHCID 6410761(Z)-Ethyl 2-(hydroxyimino)-2-(2-(tritylamino)thiazol-4-yl)acetateHCID 138082884-methylenecyclohexanol

생성물 1

HCID 140352849HCID 140352849, 화합물수율 10.5%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

4-Methylenecyclohexanol (412 mg), triphenylphosphine (860 mg), and ethyl (Z)-2-hydroxyimino-2-(2-tritylaminothiazol-4-yl)acetate (1.37 g) were dissolved together in anhydrous benzene (9 ml). Dimethyl azodicarboxylate (0.40 ml) was added slowly with stirring and the resulting orange solution was stored at room temperature for 65 h with exclusion of moisture. Workup and chromatography as in example 4a, method 3 afforded the title compound (174 mg), δH (CDCl3) 1.33 (3H, t, J 7 Hz), 1.82, 2.08 and 2.31 (8H, 3m), 4.35 (2H, q, J 7 Hz), 4.51 (1H, m), 4.63 (2H, s), 6.48 (1H, s), 6.96 (1H, br s, D2O exch.), and 7.30 (15H, s).

출처 및 근거

ORD 기록
ord-5304bb80168b4ec79145b98ad8b93c1d
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04816452

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