Hydrochloric Acid → HCID 178457009、化合物

HRID 80000

反応式

HRID 80000 の反応式
[CH:1]([NH2:4])([CH3:3])[CH3:2].[C:5]1([N:11]=[C:12]=[S:13])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.N1C=CC=CC=1.Br[CH2:21][C:22](OC)=[O:23].Cl>CO>[C:5]1([N:11]2[C:22](=[O:23])[CH2:21][S:13]/[C:12]/2=[N:4]\[CH:1]([CH3:3])[CH3:2])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6363IsopropylamineHCID 7673Phenyl IsothiocyanateHCID 60984Methyl bromoacetate

生成物 1

HCID 178457009HCID 178457009、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of isopropylamine (1.31 g, 22.19 mmol) in methanol (25 mL) is added portionwise phenylisothiocyanate (3.0 g, 22.19 mmol). The solution which becomes slightly warm during the addition is stirred at rt for 4 h before pyridine (2.63 g, 33.29 mmol) and methyl bromoacetate (3.39 g, 22.19 mmol) is added. The mixture is stirred for another 16 h at rt before it is poured onto 1 N aq. HCl (100 mL) and extracted with diethyl ether (150 mL). The aq. layer is neutralised by adding sat. aq. NaHCO3 and extracted with diethyl ether (4×150 mL). The organic extracts are dried over MgSO4 and evaporated. The remaining solid is suspended in diethyl ether/heptane, filtered off, washed with additional diethyl ether/heptane and dried to give 3-phenyl-2-[(Z)-isopropylimino]-thiazolidin-4-one.

後処理

  1. temperatureThe solution which becomes slightly warm during the addition
  2. additionis added
  3. extractionextracted with diethyl ether (150 mL)
  4. additionby adding sat. aq. NaHCO3
  5. extractionextracted with diethyl ether (4×150 mL)
  6. dry with materialThe organic extracts are dried over MgSO4
  7. customevaporated
  8. filtrationfiltered off
  9. washwashed with additional diethyl ether/heptane
  10. customdried

出典と根拠

ORDレコード
ord-e3b9f18d24bc48f88aa329f680ae8993
出典データセット
uspto-grants-2014_09
特許番号
USRE045174E1

関連ノート

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