Water → 1'-(5-iodo-1H-benzimidazol-2-yl)spiro[isobenzofuran-1,4'-piperidin]-3-one

HRID 413235

反応式

Cl[N:2]1[C:6]2[CH:7]=[CH:8][C:9]([I:11])=[CH:10][C:5]=2[N:4]=[CH:3]1.[NH:12]1[CH2:17][CH2:16][C:15]2([C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[C:19](=[O:26])[O:18]2)[CH2:14][CH2:13]1.O>CN1C(=O)CCC1>[I:11][C:9]1[CH:8]=[CH:7][C:6]2[NH:2][C:3]([N:12]3[CH2:17][CH2:16][C:15]4([C:25]5[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=5)[C:19](=[O:26])[O:18]4)[CH2:14][CH2:13]3)=[N:4][C:5]=2[CH:10]=1

参加物

実験手順

Heat a solution of 2 chloro-5-iodo-1H-benzimidazole (3.0 g, 10.7 mmol) and spiro[isobenzofuran-1,4′-piperidin]-3-one (2.63 g, 12.9 mmol) in dry NMP (15 mL) at 100° C. for 14 hours. Pour the cooled mixture into water (50 mL) and extract twice with EtOAc (50 mL). Wash the combined extracts with brine (30 mL), dry, and evaporate in vacuo. Purify by flash column chromatography (50% EtOAc-hexane) to obtain 1′-(5-iodo-1H-benzimidazol-2-yl)-spiro[isobenzofuran-1,4′-piperidin]-3-one as a beige solid.

後処理

extractionextract twice with EtOAc (50 mL)
washWash the combined extracts with brine (30 mL)
customdry
customevaporate in vacuo
customPurify by flash column chromatography (50% EtOAc-hexane)

出典と根拠

ORDレコード: ord-731be577f5434a21920bcaaf3d1a817d
出典データセット: uspto-grants-2003_05
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06566367B2

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