Thiodiglycol → HCID 70700035, 화합물

HRID 443089

반응식

HRID 443089 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH:14]=[C:15]([C:18]([CH3:21])([CH3:20])[CH3:19])[C:16]=1[OH:17])[CH2:8][CH2:9][C:10]([O:12]C)=[O:11])([CH3:4])([CH3:3])[CH3:2].[S:22]([CH2:26][CH2:27]O)[CH2:23][CH2:24]O.C([O-])(=O)C.C([O-])(=O)C.C([Sn+2]CCCC)CCC>>[C:1]([C:5]1[CH:6]=[C:7]([CH:14]=[C:15]([C:18]([CH3:21])([CH3:20])[CH3:19])[C:16]=1[OH:17])[CH2:8][CH2:9][C:10]([OH:12])=[O:11])([CH3:3])([CH3:4])[CH3:2].[C:1]([C:5]1[CH:6]=[C:7]([CH:14]=[C:15]([C:18]([CH3:21])([CH3:20])[CH3:19])[C:16]=1[OH:17])[CH2:8][CH2:9][C:10]([OH:12])=[O:11])([CH3:3])([CH3:4])[CH3:2].[S:22]([CH:26]=[CH2:27])[CH:23]=[CH2:24]

참가 물질

4

반응물 3

HCID 5447ThiodiglycolHCID 62603Methyl di-t-butyl hydroxyhydrocinnamateHCID 9798523Di-n-butyl diacetoxy tin

생성물 1

HCID 70700035HCID 70700035, 화합물

반응 조건

온도
120 °C

실험 절차

Using the general procedure of Example 11, 731 g (2.5 moles) of methyl 3,5-di-tert-butyl-4-hydroxyhydrocinnamate, and 150 g (1.23 moles) of 2,2'-thiodiethanol are heated to 120° C. Then, 0.26 g of dibutyltin diacetate (Fascat® 4200, Elf-Atochem, calculated 98 ppm Sn), is added and a vacuum of <50 mm Hg is imposed . The reaction mixture is heated to 160° C. The vacuum is reduced to <5 mm Hg and the reaction mixture is heated at 160° C. for a total of 7 hours. The vacuum is broken and the temperature is reduced to 100° C. to yield the title compound after crystallization from aqueous isopropanol. The product exhibited excellent transmission >99% at 425 nm.

후처리

  1. temperatureThe reaction mixture is heated to 160° C
  2. temperaturethe reaction mixture is heated at 160° C. for a total of 7 hours
  3. customis reduced to 100° C.

출처 및 근거

ORD 기록
ord-f0fc8453344b48909a191811819c4b15
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05892097

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