3-Hydroxypropionic acid → N-[[1-(3-hydroxypropanoyl)pyrrolidin-3-yl]methyl]-N-methyl-5-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-5,8-diazaspiro[2.5]octane-8-sulfonamide

HRID 589977ノート

反応式

HRID 589977 の反応式
[CH3:1][N:2]([CH2:23][CH:24]1[CH2:28][CH2:27][NH:26][CH2:25]1)[S:3]([N:6]1[C:11]2([CH2:13][CH2:12]2)[CH2:10][N:9]([C:14]2[C:15]3[CH:22]=[CH:21][NH:20][C:16]=3[N:17]=[CH:18][N:19]=2)[CH2:8][CH2:7]1)(=[O:5])=[O:4].CCN(C(C)C)C(C)C.[OH:38][CH2:39][CH2:40][C:41](O)=[O:42].C1CN([P+](Br)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F>CS(C)=O>[OH:42][CH2:41][CH2:40][C:39]([N:26]1[CH2:27][CH2:28][CH:24]([CH2:23][N:2]([CH3:1])[S:3]([N:6]2[C:11]3([CH2:13][CH2:12]3)[CH2:10][N:9]([C:14]3[C:15]4[CH:22]=[CH:21][NH:20][C:16]=4[N:17]=[CH:18][N:19]=3)[CH2:8][CH2:7]2)(=[O:4])=[O:5])[CH2:25]1)=[O:38]

参加物

6

反応物 4

HCID 681523-Hydroxypropionic acidHCID 81531DiisopropylethylamineHCID 2733179PyBroPHCID 57410097N-methyl-N-(pyrrolidin-3-ylmethyl)-5-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-5,8-diazaspiro[2.5]octane-8-sulfonamide2 回

生成物 1

HCID 57411295N-[[1-(3-hydroxypropanoyl)pyrrolidin-3-yl]methyl]-N-methyl-5-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-5,8-diazaspiro[2.5]octane-8-sulfonamide

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
40 °C

実験手順

N-methyl-N-(pyrrolidin-3-ylmethyl)-5-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-5,8-diazaspiro[2.5]octane-8-sulfonamide (intermediate 25) (0.042 mmol) was dissolved in dry DMSO (0.5 mL), added DIPEA (0.25 mL), 3-hydroxypropanoic acid (0.050 mmol) and Pybrop (0.050 mmol) then stirred at 40° C. for 1 h. The pure compound was obtained by standard preparative HPLC purification of the reaction mixture.

後処理

  1. customThe pure compound was obtained by standard preparative HPLC purification of the reaction mixture

出典と根拠

ORDレコード
ord-bd92120cc44c44c4af45ba052783ba1e
出典データセット
uspto-grants-2016_01
特許番号
US09233964B2

反応ノート

読み込み中…