Triethylamine → 2-Cyanoethoxy(4,5-dichloroimidazolyl)pyrrolidinophosphine

HRID 1250986ノート

反応式

HRID 1250986 の反応式
[Cl:1][C:2]1[N:3]=[CH:4][NH:5][C:6]=1[Cl:7].C(N(CC)CC)C.Cl[P:16]([O:22][CH2:23][CH2:24][C:25]#[N:26])[N:17]1[CH2:21][CH2:20][CH2:19][CH2:18]1>C(Cl)Cl>[C:25]([CH2:24][CH2:23][O:22][P:16]([C:4]1[NH:3][C:2]([Cl:1])=[C:6]([Cl:7])[N:5]=1)[N:17]1[CH2:21][CH2:20][CH2:19][CH2:18]1)#[N:26]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 1400184,5-DichloroimidazoleHCID 18325653Chloro(2-Cyanoethoxy) pyrrolidinophosphine

生成物 1

HCID 183256522-Cyanoethoxy(4,5-dichloroimidazolyl)pyrrolidinophosphine収率 82%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred solution of 4,5-dichloroimidazole (1.59 g, 11.63 mmol) and triethylamine (1.95 mL, 1.41 g, 13.96 mmol) in CH2Cl2 (30 mL) was added dropwise Chloro(2-Cyanoethoxy) pyrrolidinophosphine (2.40 g, 11.63 mmol) in CH2Cl2 (10 mL) at room temperature. The mixture was stirred for 4 h at room temperature. The reaction mixture was filtered to remove the resulting salt, and the solvent was removed under reduced pressure to give the crude product as a pale yellow oil (2.93 g, 82%). 31P NMR (CDCl3) δ 123.2.

後処理

  1. filtrationThe reaction mixture was filtered
  2. customto remove the resulting salt
  3. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-b03eb36065c84d98b1929afdb42351e3
出典データセット
uspto-grants-2002_01
特許番号
US06340749B1

反応ノート

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