Triethylamine → HCID 19600240、化合物

HRID 611255ノート

反応式

HRID 611255 の反応式
[O:1]1[C:5]2[CH2:6][NH:7][CH2:8][CH2:9][C:4]=2[CH:3]=[C:2]1[C:10]([O:12][CH3:13])=[O:11].[C:14]([C:22]1[CH:30]=[CH:29][C:25]([C:26](O)=[O:27])=[CH:24][CH:23]=1)(=[O:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C.C(P(=O)(OCC)OCC)#N>ClCCl>[C:14]([C:22]1[CH:23]=[CH:24][C:25]([C:26]([N:7]2[CH2:8][CH2:9][C:4]3[CH:3]=[C:2]([C:10]([O:12][CH3:13])=[O:11])[O:1][C:5]=3[CH2:6]2)=[O:27])=[CH:29][CH:30]=1)(=[O:21])[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 691474-Benzoylbenzoic acidHCID 76257Diethyl cyanophosphonateHCID 19600098Methyl 4,5,6,7-tetrahydrofuro[2,3-c]pyridine-2-carboxylate

生成物 1

HCID 19600240HCID 19600240、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 72 mg (0.40 mmol) of methyl 4,5,6,7-tetrahydrofuro[2,3-c]pyridin-2-carboxylate, 0.11 g (0.48 mmol) of 4-benzoylbenzoic acid and 0.11 ml (0.79 mmol) of triethylamine in 30 ml of dichloromethane, 0.07 ml (0.48 mmol) of diethyl cyanophosphonate was added dropwise at room temperature, followed by overnight stirring. After the reaction mixture was evaporated under reduced pressure, the resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=3/1 to 1/1) to yield the desired product.

後処理

  1. customAfter the reaction mixture was evaporated under reduced pressure
  2. customthe resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=3/1 to 1/1)

出典と根拠

ORDレコード
ord-5b6258c816434dd9bbb6120e933332e1
出典データセット
uspto-grants-1999_12
特許番号
US05998433

反応ノート

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