Hydrochloric Acid → HCID 53654790, 화합물

HRID 1730732노트

반응식

HRID 1730732 반응식
[CH3:1][O:2][C:3](=[O:6])[CH2:4][SH:5].[K].Cl[CH:9]([C:12]1[CH:17]=[CH:16][C:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[F:24])=[CH:14][CH:13]=1)[CH2:10][CH3:11].FC1C=CC=CC=1C1C=CC(CCC(CCC2C=CC(C3C=CC=CC=3F)=CC=2)=O)=CC=1.[BH4-].[Na+].OC(C1C=CC(C2C=CC=CC=2F)=CC=1)CC.Cl>CN(C)C=O.C1C=CC=CC=1.C(OCC)(=O)C.O>[CH3:1][O:2][C:3](=[O:6])[CH2:4][S:5][CH:9]([C:12]1[CH:17]=[CH:16][C:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[F:24])=[CH:14][CH:13]=1)[CH2:10][CH3:11]

참가 물질

12

반응물 7

HCID 313Hydrochloric AcidHCID 16907Methyl ThioglycolateHCID 27411701-(2'-Fluoro[1,1'-biphenyl]-4-yl)propan-1-olHCID 27816854-(1-chloropropyl)-2'-fluoro-1,1'-biphenylHCID 4311764Sodium borohydrideHCID 5462222PotassiumHCID 53921419HCID 53921419, 화합물

생성물 1

HCID 53654790HCID 53654790, 화합물

시약·촉매·용매 4

HCID 241Benzene용매HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

101.5 gm (0.905 mol) of potassium tert.butylate, suspended in 500 ml of dimethylformamide, were admixed, while stirring and cooling under exclusion of air, with 96.0 gm (0.905 mol) of thioglycolic acid methyl ester. To the solution of the potassium salt, the mixture was admixed with 205.9 gm (0.822 mol) of 1-chloro-1-(2'-fluoro-4-biphenylyl)-propane [prepared by reduction of 2'-fluoro-4-biphenylyl-ethylketone with sodium borohydride and subsequent reaction of the obtained 1-hydroxy-1-(2'-fluoro-4-biphenylyl)-propane with hydrochloric acid in benzene], and the mixture was stirred for 4 hours at room temperature. Subsequently, 2 liters of water were added, and the reaction product was isolated by extraction with ethyl acetate, and washing, drying and evaporating of the extract. Yield: 254 gm (97% of theory); oil, Rf -value: 0.5 (cyclohexane-ethyl acetate = 9:1 on silicagelpolygram-plates).

후처리

  1. stirringwas stirred for 4 hours at room temperature
  2. washwashing
  3. customdrying
  4. customevaporating of the extract

출처 및 근거

ORD 기록
ord-b756828650564546ac5664c2b875584c
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03993683

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