2-Methylaziridine → HCID 14013828、化合物

HRID 255435

反応式

HRID 255435 の反応式
Cl[C:2]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[C:6]([C:12]([Cl:15])([F:14])[F:13])[N:5]=[C:4]([C:16]([F:19])([F:18])[F:17])[C:3]=1[C:20]([O:22][CH2:23][CH3:24])=[O:21].C([N:27]([CH2:30][CH3:31])[CH2:28]C)C.C([O-])([O-])=O.[K+].[K+].CC1NC1>O.CN(C=O)C>[Cl:15][C:12]([F:14])([F:13])[C:6]1[N:5]=[C:4]([C:16]([F:17])([F:19])[F:18])[C:3]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[C:2]([N:27]2[CH2:28][CH:30]2[CH3:31])[C:7]=1[C:8]([O:10][CH3:11])=[O:9]

参加物

7

反応物 4

HCID 63772-MethylaziridineHCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 140137593-Ethyl 5-methyl 4-chloro-6-(chlorodifluoromethyl)-2-(trifluoromethyl)-3,5-pyridinedicarboxylate

生成物 1

HCID 14013828HCID 14013828、化合物収率 76.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To 50 ml of DMF was added 5.0 g (0.0126 mol) of product of Example 28, followed by 1.27 g (0.0126 mol) of triethylamine and 1.74 g (0.0126 mol) of K2CO3. To this mixture was added 0.922 g (0.0161 mol) of propyleneimine. This reaction mixture was stirred under N2 for 48 hours at room temperature. The reaction mixture was then poured into H2O and extracted with diethyl ether. The ether phase was then washed with H2O, and dried over MgSO4. The dry ether phase was then concentrated in vacuo to a crude yield of 4.8 g of a brown oil. This oil was kugelrohr distilled at 105° C./53 Pa, to yield 4.0 g of a yellow oil (76%) nD25 1 4763.

後処理

  1. extractionextracted with diethyl ether
  2. washThe ether phase was then washed with H2O
  3. dry with materialdried over MgSO4
  4. concentrationThe dry ether phase was then concentrated in vacuo to a crude yield of 4.8 g of a brown oil
  5. distillationThis oil was kugelrohr distilled at 105° C./53 Pa

出典と根拠

ORDレコード
ord-d3a14a3b8a0c4165a31ac5e41c94fc5f
出典データセット
uspto-grants-1987_10
特許番号
US04698093

関連ノート

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