Dimethyl Sulfoxide → HCID 70020694、化合物

HRID 397992

反応式

HRID 397992 の反応式
Cl[C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[C@H:11]2[C@H:15]([OH:16])[C@H:14]([OH:17])[C@@H:13]([C:18]3[O:22][N:21]=[C:20]([CH2:23][CH2:24][CH3:25])[N:19]=3)[O:12]2)=[C:4]([NH:26][CH2:27][CH:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[N:3]=1.[CH3:41][N:42]1[CH:46]=[C:45]([CH2:47][CH2:48][NH2:49])[N:44]=[CH:43]1.CS(C)=[O:52]>C(N(C(C)C)CC)(C)C>[CH:18]([OH:22])=[O:52].[C:35]1([CH:28]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH2:27][NH:26][C:4]2[N:3]=[C:2]([NH:49][CH2:48][CH2:47][C:45]3[N:44]=[CH:43][N:42]([CH3:41])[CH:46]=3)[N:10]=[C:9]3[C:5]=2[N:6]=[CH:7][N:8]3[C@H:11]2[C@H:15]([OH:16])[C@H:14]([OH:17])[C@@H:13]([C:18]3[O:22][N:21]=[C:20]([CH2:23][CH2:24][CH3:25])[N:19]=3)[O:12]2)[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=1

参加物

5

反応物 3

HCID 679Dimethyl SulfoxideHCID 36141-Methylhistamine2 回HCID 56624011HCID 56624011、化合物

生成物 1

HCID 70020694HCID 70020694、化合物

試薬・触媒・溶媒 1

HCID 81531Diisopropylethylamine溶媒

反応条件

温度
85 °C

実験手順

A mixture of Intermediate 23 (0.075 g, 0.135 mmol), and 2-(1-methyl-1H-imidazol-4-yl)ethylamine (0.085 g, 0.677 mmol) in diisopropylethylamine (0.04 ml) and DMSO (0.04 ml), in a sealed vial (e.g. Reacti-vial™) was heated at 85° C. for 40 h. A further portion of 2-(1-methyl-1H-imidazol-4-yl)ethylamine (0.085 g, 0.677 mmol) was added after the first 20 h. Purification by Autoprep. HPLC afforded the title compound after freeze drying as a cream solid (0.037 g). LC/MS system B Rt=2.71 mins, m/z=651 MH+

後処理

  1. customPurification by Autoprep

出典と根拠

ORDレコード
ord-6a2cee94268749dc8854975ee901a27a
出典データセット
uspto-grants-2003_08
特許番号
US06610665B1

関連ノート

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