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Water → HCID 54297194, 화합물

HRID 1277850
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HRID 1277850 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:17])[C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[C:11]([CH3:16])[CH:10]=2)=[CH:4][CH:3]=1.[SH:18][CH2:19][CH2:20][OH:21].C([O-])([O-])=O.[K+].[K+].O>CC(N(C)C)=O>[OH:21][CH2:20][CH2:19][S:18][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:17])[C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[C:11]([CH3:16])[CH:10]=2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 15672-MercaptoethanolHCID 11430Potassium CarbonateHCID 27574824-Chloro-3',4'-dimethylbenzophenone

생성물 1

HCID 54297194HCID 54297194, 화합물

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

12.2 g (0.05 mol) of 4'-chloro-3,4-dimethylbenzophenone and 4.3 g (0.055 mol) of 2-mercaptoethanol in 50 ml of dimethylacetamide are heated to 95° under nitrogen. 13.8 g (0.1 mol) of calcined K2CO3 are then added. The suspension is kept at 90°-100° C. for 6 hours. 100 ml of water are poured over the resulting reaction mixture and the mixture is extracted with ether. The ether layer is washed with water, dried over Na2SO4 and concentrated. The crystals obtained are recrystallised from methanol and dried in vacuo at 60° C. Yield: 10.1 g (71%). Melting point 92°-93° C.

후처리

  1. extractionthe mixture is extracted with ether
  2. washThe ether layer is washed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customThe crystals obtained
  6. customare recrystallised from methanol
  7. customdried in vacuo at 60° C

출처 및 근거

ORD 기록
ord-10ed8ce58d234282adf42f93a61b5743
출처 데이터셋
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04279721

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