Putrescine → Benzyl N-(4-aminobutyl)carbamate

HRID 978428노트

반응식

HRID 978428 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][NH2:6].Cl[C:8]([O:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[O:9]>C(Cl)Cl>[CH2:11]([O:10][C:8]([NH:1][CH2:2][CH2:3][CH2:4][CH2:5][NH2:6])=[O:9])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

4

반응물 2

HCID 1045PutrescineHCID 10387Benzyl chloroformate

생성물 1

HCID 2783677Benzyl N-(4-aminobutyl)carbamate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 147 g of 1,4-diaminobutane in 490 ml of methylene chloride, a solution of 41 ml of benzyl chloroformate in 84 ml of methylene chloride was added dropwise at 0° over a period of 1 hour. The mixture was stirred at 0° for 1 hour, then washed twice with water and extracted four times with 150 ml of 4N hydrochloric acid. The acidic extracts were washed with methylene chloride, basified with 450 ml of 22% of sodium hydroxide and extracted four times with methylene chloride. The organic extracts were dried over magnesium sulfate and evaporated to give 4-benzyloxycarbonylamino-1-butylamine, having NMR peaks at δ=7.3, 5.05 and 2.6 ppm.

후처리

  1. washwashed twice with water
  2. extractionextracted four times with 150 ml of 4N hydrochloric acid
  3. washThe acidic extracts were washed with methylene chloride
  4. extractionextracted four times with methylene chloride
  5. dry with materialThe organic extracts were dried over magnesium sulfate
  6. customevaporated

출처 및 근거

ORD 기록
ord-caa613fa438241b0b38016edaf104204
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04665087

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