Diphenylacetic Acid → HCID 2877827、化合物

HRID 1818086ノート

反応式

HRID 1818086 の反応式
[C:1]1([CH:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8]([OH:10])=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:17][O:18][C:19]1[CH:20]=[C:21]([C:27]2([CH2:32][NH2:33])[CH2:31][CH2:30][CH2:29][CH2:28]2)[CH:22]=[CH:23][C:24]=1[O:25][CH3:26].C(N(CC)CC)C.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1>C(#N)C>[CH3:17][O:18][C:19]1[CH:20]=[C:21]([C:27]2([CH2:32][NH:33][C:8](=[O:10])[CH:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH2:28][CH2:29][CH2:30][CH2:31]2)[CH:22]=[CH:23][C:24]=1[O:25][CH3:26]

参加物

6

反応物 4

HCID 8333Diphenylacetic AcidHCID 8471TriethylamineHCID 739193STK362959HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

生成物 1

HCID 2877827HCID 2877827、化合物収率 15.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Diphenyl-acetic acid (42.4 mg, 0.200 mmol) and C-[1-(3,4-Dimethoxy-phenyl)-cyclopentyl]-methylamine (47.1 g, 0.200 mmol) were dissolved in acetonitrile (1 mL) containing triethylamine (83.6 μL, 0.600 mmol). O-(7-Azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (76.0 mg, 0.200 mmol) was added and the solution was allowed to stir for 16 hours. The mixture was then purified by reverse phase preparative liquid chromatography to yield the pure product (13.3 mg, 0.0310 mmol, 15.5%) ESI-MS m/z calc. 429.2, found 430.2 (M+1)+. Retention time of 3.47 minutes.

後処理

  1. customThe mixture was then purified by reverse phase preparative liquid chromatography

出典と根拠

ORDレコード
ord-3b9b2f6f96e2413e904d4c69ef6ce9e4
出典データセット
uspto-grants-2009_10
特許番号
US07598412B2

反応ノート

読み込み中…