Methanol → 4-(4,8,11-Tris-(2,2,2-trifluoroacetyl)-1,4,8,11-tetraazacyclotetradec-1-ylmethyl)-benzoic acid

HRID 507797

反応式

[N:1]1([CH2:15][C:16]2[CH:24]=[CH:23][C:19]([C:20]([OH:22])=[O:21])=[CH:18][CH:17]=2)[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9][NH:8][CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[CH3:25][OH:26].[F:27][C:28]([F:35])([F:34])[CH2:29][O:30]C(=O)C>C(N(CC)CC)C>[F:35][C:28]([F:27])([F:34])[C:29]([N:4]1[CH2:5][CH2:6][CH2:7][N:8]([C:25](=[O:26])[C:28]([F:35])([F:34])[F:27])[CH2:9][CH2:10][N:11]([C:29](=[O:30])[C:28]([F:35])([F:34])[F:27])[CH2:12][CH2:13][CH2:14][N:1]([CH2:15][C:16]2[CH:24]=[CH:23][C:19]([C:20]([OH:22])=[O:21])=[CH:18][CH:17]=2)[CH2:2][CH2:3]1)=[O:30]

参加物

実験手順

To a two-neck round bottom flask purged with argon was added successively 4-(1,4,8,11-tetraazacyclotetradec-1-ylmethyl)-benzoic acid (90 mg, 0.24 mmol), dry methanol (1 ml), dry triethyl amine (0.5 ml) and trifluoroethylacetate (1.7 ml). All following procedures were carried on in argon atmosphere. The mixture was stirred for 60 hours. After that the solvents were removed at reduced pressure and the residue was taken up in dry tetrahydrofurane (5 ml). The THF solution was filtered and the solvent removed at reduced pressure. The residue was dried in vacuo for 4 hours to produce 0.54 g of oily compound. MS m/z 623.5 M[C24H27F9N4O5]+1.

後処理

customTo a two-neck round bottom flask purged with argon
customAfter that the solvents were removed at reduced pressure
filtrationThe THF solution was filtered
customthe solvent removed at reduced pressure
customThe residue was dried in vacuo for 4 hours

出典と根拠

ORDレコード: ord-7e80c693879d4ac3860835df41c536e3
出典データセット: uspto-grants-2010_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07786292B2

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

関連ノート