홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

4-Methylpentane-1,2-diol → 2,5-Di(p-toluidino)-terephthalic acid dimethyl ester

HRID 2226284
노트
인쇄 미리보기

반응식

HRID 2226284 반응식
[CH3:1][O:2][C:3](=[O:30])[C:4]1[CH2:13][C:12]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=2)=[C:7]([C:8]([O:10][CH3:11])=[O:9])[CH2:6][C:5]=1[NH:22][C:23]1[CH:28]=[CH:27][C:26]([CH3:29])=[CH:25][CH:24]=1.CC(CC(O)CO)C>[Mo].C1(C)C(C)=CC=CC=1>[CH3:11][O:10][C:8](=[O:9])[C:7]1[CH:6]=[C:5]([NH:22][C:23]2[CH:28]=[CH:27][C:26]([CH3:29])=[CH:25][CH:24]=2)[C:4]([C:3]([O:2][CH3:1])=[O:30])=[CH:13][C:12]=1[NH:14][C:15]1[CH:16]=[CH:17][C:18]([CH3:21])=[CH:19][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 911714-Methylpentane-1,2-diolHCID 1171141,4-Cyclohexadiene-1,4-dicarboxylic acid, 2,5-bis[(4-methylphenyl)amino]-, 1,4-dimethyl ester

생성물 1

HCID 197652112,5-Di(p-toluidino)-terephthalic acid dimethyl ester

시약·촉매·용매 2

HCID 23932Molybdenum촉매HCID 7237O-Xylene용매

실험 절차

0.1-0.8 part of molybdenum or vanadium(IV) oxide acetyl-acetonate is then added as a catalyst, or a V4A wire gauze is wound around the stirrer. A stream of air, preheated if appropriate, of about 15 liters per hour is then introduced through an immersed tube at a temperature of 103° C. for about 8-9 hours. The stream of waste gas is passed over a separator for the water of reaction, over a cooler and over a washing column, for example with polyethylene glycol dimethyl ether, for absorption of xylene emissions. The current concentration of the oxygen is measured in the stream of waste gas. It is about 15% by volume on average. In this apparatus arrangement, the oxygen content of the air is utilized to the extent of about 25%. Samples are taken hourly for liquid chromatography (HPLC), and a conversion curve, expressed in percent by weight, of starting material and product is thus plotted. The 1st derivation (angle of the tangents) should decrease constantly from about 50% of the conversion. About 20% of the xylene (149 parts with 24 parts of propionic acid) is then distilled off. The remaining majority of the xylene is then distilled off by steam distillation, an aqueous suspension of 2,5-di-p-toluidino-terephthalic acid dimethyl ester finally being obtained. The xylene removed by steam distillation is purified and used for the preparation of the SucEst. The 2,5-di-p-toluidino-terephthalic acid dimethyl ester is isolated by filtration over a heated pressure suction filter (preferably fitted with a stirrer). The crystal-line crude product (226 parts by weight, melting point 205°-207° C.) on the suction filter is blown out with steam until it is odorless. It is then washed with methanol. 195 parts of methanol-moist 2,5-di-p-toluidino-terephthalic acid dimethyl ester (=97% of theory, based on the SucEst,) of melting point 215°-220° C. are obtained.

후처리

  1. additionis then introduced through an immersed tube at a temperature of 103° C. for about 8-9 hours
  2. concentrationThe current concentration of the oxygen
  3. distillationAbout 20% of the xylene (149 parts with 24 parts of propionic acid) is then distilled off
  4. distillationThe remaining majority of the xylene is then distilled off by steam distillation
  5. additionan aqueous suspension of 2,5-di-p-toluidino-terephthalic acid dimethyl ester
  6. customfinally being obtained
  7. customThe xylene removed by steam distillation
  8. customis purified
  9. customused for the preparation of the SucEst

출처 및 근거

ORD 기록
ord-d56d20a398f6457b9c1380347daab437
출처 데이터셋
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05347038

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트