Hydrochloric Acid → 3,5-dichloro-2-amino-N-(2-hydroxyethoxy)benzamide

HRID 558067

반응식

HRID 558067 반응식
[Cl:1][C:2]1[C:3]([NH2:13])=[C:4]([CH:9]=[C:10]([Cl:12])[CH:11]=1)[C:5]([O:7]C)=O.[NH2:14][O:15][CH2:16][CH2:17][OH:18].C[O-].[Na+].Cl>CO.O>[Cl:1][C:2]1[C:3]([NH2:13])=[C:4]([CH:9]=[C:10]([Cl:12])[CH:11]=1)[C:5]([NH:14][O:15][CH2:16][CH2:17][OH:18])=[O:7]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 613050Methyl 2-amino-3,5-dichlorobenzoateHCID 3014186Ethanol, 2-(aminooxy)-HCID 10942334Sodium Methoxide

생성물 1

HCID 866307723,5-dichloro-2-amino-N-(2-hydroxyethoxy)benzamide

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

9 g (40.9 mmol) of methyl 3,5-dichloro-2-aminobenzoate and 6.3 g (81.8 mmol) of 2-(aminooxy)ethanol are initially charged in 90 ml of methanol, and 22.1 g (122.7 mmol) of sodium methoxide as a 30% strength solution in methanol are added dropwise at 20° C. The mixture is stirred at 50° C. overnight. The mixture is cooled and poured onto 400 ml of water, and the pH is adjusted to 3 using 1 N hydrochloric acid. The mixture is extracted 3 times with in each case 150 ml of ethyl acetate and the extracts are dried with sodium sulphate and concentrated using a rotary evaporator.

후처리

  1. temperatureThe mixture is cooled
  2. extractionThe mixture is extracted 3 times with in each case 150 ml of ethyl acetate
  3. dry with materialthe extracts are dried with sodium sulphate
  4. concentrationconcentrated
  5. customa rotary evaporator

출처 및 근거

ORD 기록
ord-f392fc23c3624e0bbbb713a5ea5747e4
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08062995B2

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