1-Hydroxybenzotriazole → HCID 15435300、化合物

HRID 617647ノート

反応式

HRID 617647 の反応式
[CH2:1]([O:8][C:9]([NH:11][C:12]1[C:17](=[O:18])[N:16]([CH2:19][C:20](O)=[O:21])[C:15]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[N:14][CH:13]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:29][CH:30]([CH2:37][C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)[CH:31]([OH:36])[C:32]([F:35])([F:34])[F:33].CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C>[CH2:1]([O:8][C:9]([NH:11][C:12]1[C:17](=[O:18])[N:16]([CH2:19][C:20]([NH:29][CH:30]([CH2:37][C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[C:31](=[O:36])[C:32]([F:33])([F:34])[F:35])=[O:21])[C:15]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[N:14][CH:13]=1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 102491135-benzyloxycarbonylamino-6-oxo-2-phenyl-1,6-dihydropyrimidin-1-ylacetic acidHCID 145032493-Amino-1,1,1-trifluoro-4-phenylbutan-2-ol

生成物 1

HCID 15435300HCID 15435300、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of (5-benzyloxycarbonylamino-6-oxo-2-phenyl-1,6-dihydro-1-pyrimidinyl)acetic acid (title compound in Reference Example 2, 8.57 g, 22.6 mmol) and 3-amino-1,1,1-trifluoro-4-phenyl-2-butanol (title compound in Reference Example 1, 5.91 g, 27.2 mmol) in DMF (75 mL) were added WSCI hydrochloride (5.20 g, 27.2 mmol) and HOBT (6.10 g, 45.1 mmol). The resulting mixture was stirred at room temperature for 16 h, poured into 0.5N hydrochloric acid (500 mL), and then extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogencarbonate solution and saturated brine, and dried over anhydrous magnesium sulfate. The residue obtained by concentration of the extract was separated and purified by silica gel column chromatography (chloroform-ethyl acetate, 83:17) to give 11.4 g (87%) of 2-(5-benzyloxycarbonylamino-6-oxo-2-phenyl-1,6-dihydro-1-pyrimidyl)-N-(1-benzyl-3,3,3-trifluoro-2-hydroxypropyl)-acetamide as colorless crystals.

出典と根拠

ORDレコード
ord-b72884d3497e4f6781d6c55879cc45a7
出典データセット
uspto-grants-1999_09
特許番号
US05948785

反応ノート

読み込み中…