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Benzene, 1-isocyanato-2-methoxy- → 1-(2-Methoxyphenyl)-3-(2,4,6-trimethyl-3-pyrrolidin-1-yl-phenyl)-urea

HRID 2251309
ノート
印刷プレビュー

反応式

HRID 2251309 の反応式
[CH3:1][C:2]1[C:7]([N:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)=[C:6]([CH3:13])[CH:5]=[C:4]([CH3:14])[C:3]=1[NH2:15].[CH3:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[N:24]=[C:25]=[O:26]>C1(C)C=CC=CC=1.CCOC(C)=O>[CH3:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[NH:24][C:25]([NH:15][C:3]1[C:4]([CH3:14])=[CH:5][C:6]([CH3:13])=[C:7]([N:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)[C:2]=1[CH3:1])=[O:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 69695Benzene, 1-isocyanato-2-methoxy-HCID 107982512,4,6-Trimethyl-3-(pyrrolidin-1-yl)aniline

生成物 1

HCID 596436591-(2-Methoxyphenyl)-3-(2,4,6-trimethyl-3-pyrrolidin-1-yl-phenyl)-urea収率 25.5%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 2 (0.25 g, 1.22 mmol) and 2-methoxyphenyl isocyanate (0.18 g, 1.22 mmol) in toluene (5 mL) was heated at 80° C. overnight. The mixture was allowed to cool to room temperature and then diluted with EtOAc. The organic layer was washed with water (50 mL) and brine (50 mL) before it was dried (MgSO4) and concentrated on a rotavap. The residue was chromatographed on silica gel to give the title compound (0.11 g) as a solid. ESI [M+H+]=354.22.

後処理

  1. washThe organic layer was washed with water (50 mL) and brine (50 mL) before it
  2. dry with materialwas dried (MgSO4)
  3. concentrationconcentrated on a rotavap
  4. customThe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-442fdc50fb264519892896a0f28a9c40
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07319111B2

反応ノート

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