Formaldehyde → Tert-butyl 4-[(5-chloro-6-hydroxy-3-oxo-2,3-dihydrobenzofuran-7-yl)methyl]piperazine-1-carboxylate

HRID 1749711ノート

反応式

HRID 1749711 の反応式
[Cl:1][C:2]1[C:3]([OH:12])=[CH:4][C:5]2[O:9][CH2:8][C:7](=[O:10])[C:6]=2[CH:11]=1.[C:13]([O:17][C:18]([N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1)=[O:19])([CH3:16])([CH3:15])[CH3:14].[CH2:26]=O>C(O)C>[Cl:1][C:2]1[C:3]([OH:12])=[C:4]([CH2:26][N:23]2[CH2:24][CH2:25][N:20]([C:18]([O:17][C:13]([CH3:16])([CH3:14])[CH3:15])=[O:19])[CH2:21][CH2:22]2)[C:5]2[O:9][CH2:8][C:7](=[O:10])[C:6]=2[CH:11]=1

参加物

5

反応物 3

HCID 712FormaldehydeHCID 143452tert-Butyl piperazine-1-carboxylateHCID 574435495-chloro-6-hydroxybenzofuran-3(2H)-one

生成物 1

HCID 71278506Tert-butyl 4-[(5-chloro-6-hydroxy-3-oxo-2,3-dihydrobenzofuran-7-yl)methyl]piperazine-1-carboxylate収率 56.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 5-chloro-6-hydroxybenzofuran-3(2H)-one (0.185 g, 1.00 mmol) in ethanol (20 mL) was added with 1-tert-butoxycarbonylpiperazine (0.186 g, 1.00 mmol), and 37% aqueous formaldehyde (0.0812 g, 1.00 mmol) at room temperature. The mixture was stirred overnight at room temperature, and then the precipitates formed were collected by filtration, and then washed with ethyl acetate to obtain tert-butyl 4-[(5-chloro-6-hydroxy-3-oxo-2,3-dihydrobenzofuran-7-yl)methyl]piperazine-1-carboxylate (0.216 g, 56%).

後処理

  1. customthe precipitates formed
  2. filtrationwere collected by filtration
  3. washwashed with ethyl acetate

出典と根拠

ORDレコード
ord-7fbf3da338ed494fbb552cb3a247000b
出典データセット
uspto-grants-2015_10
特許番号
US09156827B2

反応ノート

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