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

HRID 1749878노트

반응식

HRID 1749878 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-c4c9dce3b15f4a3592e92c2c1fb4c3e8
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09156827B2

반응 노트

불러오는 중…