Butylamine → Guanidine, pentabutyl-

HRID 625160

反応式

HRID 625160 の反応式
[CH2:1]([N:5]([CH2:17][CH2:18][CH2:19][CH3:20])[C:6](=O)[N:7]([CH2:12][CH2:13][CH2:14][CH3:15])[CH2:8][CH2:9][CH2:10][CH3:11])[CH2:2][CH2:3][CH3:4].P(Cl)(Cl)(Cl)=O.[CH2:26]([NH2:30])[CH2:27][CH2:28][CH3:29]>C(#N)C>[CH2:1]([N:5]([CH2:17][CH2:18][CH2:19][CH3:20])[C:6](=[N:30][CH2:26][CH2:27][CH2:28][CH3:29])[N:7]([CH2:12][CH2:13][CH2:14][CH3:15])[CH2:8][CH2:9][CH2:10][CH3:11])[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 3

HCID 8007ButylamineHCID 20691TetrabutylureaHCID 24813Phosphorus oxychloride

生成物 1

HCID 189218Guanidine, pentabutyl-

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
75 °C

実験手順

A mixture of 5.69 grams (20 mmol) of tetra-n-butylurea, 3.22 grams (21 mmol) of phosphorus oxychloride and 15 ml of acetonitrile was heated at 75° C. in a nitrogen atmosphere for one hour. The mixture was then cooled to 0° C. and 3.36 grams (46 mmol) of n-butylamine was added over 15 minutes with stirring. The mixture was warmed to 60° C. for one hour and again cooled to 0° C., quenched with 5 ml of 25% (by weight) aqueous sodium hydroxide solution and extracted with diethylether. The ether extracts were dried over sodium sulphate, filtered and stripped to give a pale yellow oil of penta-n-butylguanidine.

後処理

  1. temperatureThe mixture was then cooled to 0° C.
  2. temperatureThe mixture was warmed to 60° C. for one hour
  3. temperatureagain cooled to 0° C.
  4. customquenched with 5 ml of 25% (by weight) aqueous sodium hydroxide solution
  5. extractionextracted with diethylether
  6. dry with materialThe ether extracts were dried over sodium sulphate
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-2146dd7589814ff595e4d32eb410833d
出典データセット
uspto-grants-2016_04
特許番号
US09303201B2

関連ノート

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