ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

3-(4-Hydroxyphenyl)propionic acid → N-(2,4-difluorobenzyl)-N-heptyl-3-(4-hydroxyphenyl)propanamide

HRID 899876
ノート
印刷プレビュー

反応式

HRID 899876 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10]([OH:12])=O)=[CH:4][CH:3]=1.[F:13][C:14]1[CH:28]=[C:27]([F:29])[CH:26]=[CH:25][C:15]=1[CH2:16][NH:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24].CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CCN(C(C)C)C(C)C.C(=O)([O-])O.[Na+]>CN(C=O)C.C(OCC)(=O)C>[F:13][C:14]1[CH:28]=[C:27]([F:29])[CH:26]=[CH:25][C:15]=1[CH2:16][N:17]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[C:10](=[O:12])[CH2:9][CH2:8][C:5]1[CH:4]=[CH:3][C:2]([OH:1])=[CH:7][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 103943-(4-Hydroxyphenyl)propionic acidHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 60663854N-(2,4-difluorobenzyl)-N-heptylamine

生成物 1

HCID 69120490
N-(2,4-difluorobenzyl)-N-heptyl-3-(4-hydroxyphenyl)propanamide
収率 88.1%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

3-(4-Hydroxyphenyl)propionic acid (108 mg, 0.650 mmol) was dissolved in DMF. N-(2,4-difluorobenzyl)-N-heptylamine (164.7 mg, 0.682 mmol) was added. The mixture was cooled in an ice-bath. TBTU (219 mg, 0.682 mmol) was added and followed by DIPEA (0.238 ml, 1.365 mmol). The mixture was stirred overnight and the temperature was allowed up to room temperature. Ethyl acetate and sodium hydrogencarbonate aqueous solution (sat.) were added and then the two phases were separated. The water phase was extracted with ethyl acetate. The organic phases were combined and dried with magnesium sulphate and evaporated. Chromatography of the residue on a column (ISOLUTE® SI, 5 g/15 ml) using DCM and then MeOH/DCM (1:99) as eluant gave 223 mg desired product, yield 88%.

後処理

  1. temperatureThe mixture was cooled in an ice-bath
  2. customwas allowed up to room temperature
  3. customthe two phases were separated
  4. extractionThe water phase was extracted with ethyl acetate
  5. dry with materialdried with magnesium sulphate
  6. customevaporated

出典と根拠

ORDレコード
ord-0ebb6f182eb345b38dfe864bb0f1a213
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07355069B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート