Triphenylphosphine → HCID 140352849、化合物

HRID 1194945ノート

反応式

HRID 1194945 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 140352849HCID 140352849、化合物収率 10.5%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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).

出典と根拠

ORDレコード
ord-5304bb80168b4ec79145b98ad8b93c1d
出典データセット
uspto-grants-1989_03
特許番号
US04816452

反応ノート

読み込み中…