N,N-Dimethylcyclohexylamine → Toluene 2,4-Diisocyanate

HRID 1169019

반응식

HRID 1169019 반응식
OCC1COC(=O)O1.CN(C)C1CCCCC1.[N-:18]=[C:19]=[O:20].[N-:21]=[C:22]=[O:23].[C:24]1([CH3:30])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>O1CCCC1>[CH3:30][C:24]1[C:25](=[CH:26][C:27](=[CH:28][CH:29]=1)[N:21]=[C:22]=[O:23])[N:18]=[C:19]=[O:20]

참가 물질

5

반응물 3

HCID 7415N,N-DimethylcyclohexylamineHCID 97944Glycerol carbonateHCID 21584847HCID 21584847, 화합물2회

생성물 1

HCID 11443Toluene 2,4-Diisocyanate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a one-liter, round bottom 3-necked flask, fitted with a mechanical stirrer, thermometer and dropping funnel, was added 118 g of glycerin carbonate (I) (1.0 moles) and 200 ml. of dry tetrahydofuran (THF). After addition of 1.0 g dimethylcyclohexylamine (DMCHA), the resulting solution was stirred under nitrogen at ambient temperature. Then, 87 g (1.0 equiv.) of Rubinate® 80/20 (Huntsman Corp.) toluenediisocyanate (TDI) (II) was then added dropwise while controlling the exothermic reaction so that the temperature did not exceed 60° C. After the addition of compound II was complete the reaction product was maintained at 50° C. for one hour. The resulting product was primarily a solution of III in THF, a light yellow mobile liquid. The reaction is shown diagrammatically below.

후처리

  1. customTo a one-liter, round bottom 3-necked flask, fitted with a mechanical stirrer
  2. customthe exothermic reaction so that the temperature
  3. customdid not exceed 60° C
  4. temperaturewas maintained at 50° C. for one hour

출처 및 근거

ORD 기록
ord-f9d1931a0fa0480eaa454d25ae67df20
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06627761B2

연결된 노트

불러오는 중…