Butylamine → Guanidine, pentabutyl-

HRID 625160

반응식

HRID 625160 반응식
[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]

참가 물질

5

반응물 3

HCID 8007ButylamineHCID 20691TetrabutylureaHCID 24813Phosphorus oxychloride

생성물 1

HCID 189218Guanidine, pentabutyl-

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
75 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2146dd7589814ff595e4d32eb410833d
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09303201B2

연결된 노트

불러오는 중…