Phosgene → Methyl(pentyl)carbamyl chloride

HRID 66338

反応式

HRID 66338 の反応式
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]

参加物

6

反応物 3

HCID 6371PhosgeneHCID 8471TriethylamineHCID 117479N-Methylpentylamine

生成物 1

HCID 15209943Methyl(pentyl)carbamyl chloride

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 7962Methylcyclohexane溶媒

反応条件

温度
-10 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a885dadfe7b7440faa0f634571ffd442
出典データセット
uspto-grants-1978_12
特許番号
US04131674

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