Diisopropylethylamine → HCID 68406051、化合物

HRID 1713980ノート

反応式

HRID 1713980 の反応式
[N:1]1([CH2:7][CH2:8][C:9]([OH:11])=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl([O-])(=O)(=O)=O.CN([P+](N(C)C)(N(C)C)Cl)C.C(N(CC)C(C)C)(C)C.[NH2:37][CH2:38][CH2:39][CH2:40][N:41]([C:49]1[S:50][CH:51]=[C:52]([C:54]2[O:55][C:56]3[CH:62]=[CH:61][CH:60]=[CH:59][C:57]=3[CH:58]=2)[N:53]=1)[C:42]([C:44]1[S:45][CH:46]=[CH:47][CH:48]=1)=[O:43]>CN1C(=O)CCC1>[O:55]1[C:56]2[CH:62]=[CH:61][CH:60]=[CH:59][C:57]=2[CH:58]=[C:54]1[C:52]1[N:53]=[C:49]([N:41]([CH2:40][CH2:39][CH2:38][NH:37][C:9](=[O:11])[CH2:8][CH2:7][N:1]2[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]2)[C:42]([C:44]2[S:45][CH:46]=[CH:47][CH:48]=2)=[O:43])[S:50][CH:51]=1

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 1177821-Piperidinepropanoic acidHCID 68407996N-(3-aminopropyl)-N-(4-(benzofuran-2-yl)thiazol-2-yl)thiophene-2-carboxamideHCID 86603592HCID 86603592、化合物

生成物 1

HCID 68406051HCID 68406051、化合物収率 30.6%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

A mixture of 1-piperidinepropionic acid (3 mg, 0.02 mmol) and tris(dimethylamino)chlorophosphonium perchlorate (7 mg, 0.02 mmol) was dissolved in NMP (200 μL) followed by the addition of N,N-diisopropylethylamine (17 μL, 0.1 mmol). The reaction mixture was maintained at room temperature for 20 min, then N-(3-aminopropyl)-N-(4-(benzofuran-2-yl)thiazol-2-yl)thiophene-2-carboxamide (7.7 mg, 0.02 mmol) was added, and the reaction mixture was stirred at room temperature overnight. The resulting mixture was subjected to HPLC purification (Method Z) to provide the title compound (3.2 mg) as a pale yellow solid. LC/MS (ESI) m/z 523.5 [M+H]. HPLC retention time (Method C)=3.15 min.

後処理

  1. customThe resulting mixture was subjected to HPLC purification (Method Z)

出典と根拠

ORDレコード
ord-571eb34339cc46c1b12c747c813a0e4b
出典データセット
uspto-grants-2010_09
特許番号
US07795290B2

反応ノート

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