Dimethylcarbamoyl Chloride → HCID 69748249、化合物

HRID 2181613ノート

反応式

HRID 2181613 の反応式
[CH3:1][CH:2]1[CH2:7][NH:6][CH2:5][CH:4]([CH3:8])[NH:3]1.C(N(CC)CC)C.[CH3:16][N:17]([CH3:21])[C:18](Cl)=[O:19]>C(Cl)Cl>[CH3:16][N:17]([CH3:21])[C:18]([N:3]1[CH:4]([CH3:8])[CH2:5][NH:6][CH2:7][CH:2]1[CH3:1])=[O:19]

参加物

5

反応物 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 660562,6-Dimethylpiperazine

生成物 1

HCID 69748249HCID 69748249、化合物収率 70%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To an ice-cold solution of 2,6-dimethyl piperazine (179 mmol, 20.4 g), methylene chloride (200 mL), and triethylamine (214 mmol, 29.9 mL) was added dropwise dimethylcarbamoyl chloride (179 mmol, 16.4 mL). After 4 hr the reaction was quenched with a saturated sodium bicarbonate solution and the methylene chloride layer was collected, dried, filtered and the filtrate was evaporated to dryness to obtain an orange oil, 2,6-dimethyl-piperazine-1-carboxylic acid dimethylamide (70%, 23.1 g).

後処理

  1. customAfter 4 hr the reaction was quenched with a saturated sodium bicarbonate solution
  2. customthe methylene chloride layer was collected
  3. customdried
  4. filtrationfiltered
  5. customthe filtrate was evaporated to dryness

出典と根拠

ORDレコード
ord-61765786640a449db6baee62d62d034a
出典データセット
uspto-grants-2005_05
特許番号
US06894047B2

反応ノート

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