Hydrochloric Acid → HCID 54085422, 화합물

HRID 1730739노트

반응식

HRID 1730739 반응식
[BH4-].[Na+].[CH3:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][C:14]([CH:17](O)[CH3:18])=[CH:13][CH:12]=2)=[CH:7][CH:6]=1.COC1C=CC(C2C=CC(C(Cl)C)=CC=2)=CC=1.Cl.[CH3:38][O:39][C:40](=[O:43])[CH2:41][SH:42].C(=O)([O-])[O-].[K+].[K+]>CS(C)=O.C1CCCCC1.CO>[CH3:38][O:39][C:40](=[O:43])[CH2:41][S:42][CH:17]([C:14]1[CH:15]=[CH:16][C:11]([C:8]2[CH:9]=[CH:10][C:5]([O:4][CH3:3])=[CH:6][CH:7]=2)=[CH:12][CH:13]=1)[CH3:18]

참가 물질

10

반응물 6

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 16907Methyl ThioglycolateHCID 4311764Sodium borohydrideHCID 14533349HCID 14533349, 화합물HCID 203487384-(1-Chloroethyl)-4'-methoxy-1,1'-biphenyl2회

생성물 1

HCID 54085422HCID 54085422, 화합물

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 887Methanol용매HCID 8078Cyclohexane용매

실험 절차

(4'-Methoxy-4-biphenyl)-methyl-ketone [see W. S. Johnson et al, J. Amer. Chem. Soc. 68, 1648 (1946)] was reduced with sodium borohydride to 1-(4'-methoxy-4-biphenylyl)-ethanol (m.p. 120°-122° C, from cyclohexane), and the carbinol was converted into 1-(4'-methoxy-4-biphenylyl)-1-chloroethane, m.p. 122°-124° C (from cyclohexane), with hydrogen chloride. 5.2 gm of 1-(4'-methoxy-4-biphenylyl)-1-chloroethane (0.021 mol) were admixed in 21 ml of dry dimethyl sulfoxide with 2.7 gm (0.026 mol) of thioglycolic acid methyl ester and then with 3.5 gm (0.026 mol) of dry potassium carbonate. The mixture was stirred at room temperature for 45 minutes. The reaction product was precipitated with water, suction-filtered off, washed and dried. Yield: 6.8 gm (100% of theory); m.p. 59°-61° C. A sample recrystallized from cyclohexane, analized as follows:

후처리

  1. customThe reaction product was precipitated with water
  2. filtrationsuction-filtered off
  3. washwashed
  4. customdried
  5. customA sample recrystallized from cyclohexane

출처 및 근거

ORD 기록
ord-ce26b216ca0a45ef814b994e543386e9
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03993683

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