Phosgene → Methyl(pentyl)carbamyl chloride

HRID 66338

반응식

HRID 66338 반응식
C(N(CC)CC)C.[C:8]([Cl:11])(Cl)=[O:9].[CH3:12][NH:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]>CC1CCCCC1.C1(C)C=CC=CC=1>[CH3:12][N:13]([CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[C:8]([Cl:11])=[O:9]

참가 물질

6

반응물 3

HCID 6371PhosgeneHCID 8471TriethylamineHCID 117479N-Methylpentylamine

생성물 1

HCID 15209943Methyl(pentyl)carbamyl chloride

시약·촉매·용매 2

HCID 1140Toluene용매HCID 7962Methylcyclohexane용매

반응 조건

온도
-10 °C

실험 절차

Triethylamine (14 cc.) is added over the course of 8 minutes to a 2.5N solution (42 cc.) of phosgene in methylcyclohexane, cooled to -10° C., and a solution of N-methylpentylamine (13.7 cc.) in toluene (50 cc.) is then added whilst maintaining the temperature at -10° C. The mixture is stirred for 1 hour at +5° C. The insoluble material is then filtered off and washed with toluene (80 cc.). The organic solutions are dried over calcium chloride (10 g.). After filtration, the solvents are evaporated under reduced pressure (40 mm.Hg). The residue is distilled under reduced pressure to give N-methyl-N-pentylcarbamoyl chloride (5.6 g.), b.p. 120-125° C./40 mm.Hg.

후처리

  1. temperaturewhilst maintaining the temperature at -10° C
  2. filtrationThe insoluble material is then filtered off
  3. washwashed with toluene (80 cc.)
  4. dry with materialThe organic solutions are dried over calcium chloride (10 g.)
  5. filtrationAfter filtration
  6. customthe solvents are evaporated under reduced pressure (40 mm.Hg)
  7. distillationThe residue is distilled under reduced pressure

출처 및 근거

ORD 기록
ord-a885dadfe7b7440faa0f634571ffd442
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04131674

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