Hydrochloric Acid → HCID 53654790、化合物

HRID 1730732ノート

反応式

HRID 1730732 の反応式
[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]

参加物

12

反応物 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、化合物

生成物 1

HCID 53654790HCID 53654790、化合物

試薬・触媒・溶媒 4

HCID 241Benzene溶媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-b756828650564546ac5664c2b875584c
出典データセット
uspto-grants-1976_11
特許番号
US03993683

反応ノート

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