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Ethylene Glycol → HCID 57166565, 화합물

HRID 256394
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HRID 256394 반응식
[CH:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[S:9](=[O:14])(=[O:13])[CH2:8][CH2:7][CH2:6]2)=[O:2].C1(C)C=CC=CC=1.[CH2:22](O)[CH2:23][OH:24].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>O>[O:2]1[CH2:22][CH2:23][O:24][CH:1]1[C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[S:9](=[O:14])(=[O:13])[CH2:8][CH2:7][CH2:6]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 1140TolueneHCID 521998p-Toluenesulfonic acid monohydrateHCID 137287301,1-dioxo-3,4-dihydro-2H-1lambda6-benzothiopyran-6-carbaldehyde

생성물 1

HCID 57166565HCID 57166565, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of 3.0 g (14.3 mmole) 6-formyl-1,1dioxothiachroman and 140 ml toluene was added 15.9 ml ethylene glycol and 0.66 g (3.5 mmole) p-toluenesulfonic acid hydrate. The mixture was heated at reflux for 18 hours or until no further water was collected in the attached water separator (Dean-Stark trap). The reaction mixture was cooled, diluted with ethyl acetate, washed with water, sodium bicarbonate, water again, brine and dried (MgSO4). Evaporation of solvent in vacuo gave 3.73 g of residual oil which solidified on standing. Mass spectrum (m/e): 254 (M+).

후처리

  1. temperatureThe mixture was heated
  2. customwas collected in the attached water separator (Dean-Stark trap)
  3. temperatureThe reaction mixture was cooled
  4. additiondiluted with ethyl acetate
  5. washwashed with water, sodium bicarbonate, water again
  6. dry with materialbrine and dried (MgSO4)
  7. customEvaporation of solvent in vacuo

출처 및 근거

ORD 기록
ord-90ab59e28b6944999f0abd62c09bedaa
출처 데이터셋
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04703052

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