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Potassium Carbonate → 3-{1-[2-[(4-Chlorobenzoyl)amino]ethyl]-2-pyrrolidinyl}phenyl methylcarbamate

HRID 1654032
ノート
印刷プレビュー

反応式

HRID 1654032 の反応式
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]([C:6]([NH:8][CH2:9][CH2:10][N:11]2[CH2:15][CH2:14][CH2:13][CH:12]2[C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([OH:22])[CH:17]=2)=[O:7])=[CH:4][CH:3]=1.[CH3:25][N:26]=[C:27]=[O:28].C(=O)([O-])[O-].[K+].[K+]>O1CCCC1>[CH3:25][NH:26][C:27](=[O:28])[O:22][C:18]1[CH:19]=[CH:20][CH:21]=[C:16]([CH:12]2[CH2:13][CH2:14][CH2:15][N:11]2[CH2:10][CH2:9][NH:8][C:6](=[O:7])[C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:24][CH:23]=2)[CH:17]=1
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 3

HCID 11430Potassium CarbonateHCID 12228Methyl IsocyanateHCID 233612984-chloro-N-{2-[2-(3-hydroxyphenyl)-1-pyrrolidinyl]ethyl}benzamide

生成物 1

HCID 152227993-{1-[2-[(4-Chlorobenzoyl)amino]ethyl]-2-pyrrolidinyl}phenyl methylcarbamate収率 94%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The 4-chloro-N-{2-[2-(3-hydroxyphenyl)-1-pyrrolidinyl]ethyl}benzamide (0.29 g) was dissolved in tetrahydrofuran (20 ml), and methyl isocyanate (50.0 μl) and milled potassium carbonate (0.17 g) at ambient temperature were added, under nitrogen. The reaction mixture was stirred for 2 hrs and filtered through a pad of celite. The filter cake was washed with ethyl acetate, and the combined filtrates were concentrated. Crystallization of the residue with ether/petroleum ether gave 0.32 g (94%) of product. Recrystallization from ether gave the analytical sample, mp 103°-106° C.

後処理

  1. additionwere added, under nitrogen
  2. filtrationfiltered through a pad of celite
  3. washThe filter cake was washed with ethyl acetate
  4. concentrationthe combined filtrates were concentrated
  5. customCrystallization of the residue with ether/petroleum ether

出典と根拠

ORDレコード
ord-aebbf3b608394fc99accae981a82d03b
出典データセット
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05405845

反応ノート

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