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Water → [2-(2-Thienyl)ethylamino](2-chlorophenyl)acetamide

HRID 568125
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HRID 568125 반응식
Cl.[S:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH2:7][CH2:8][NH:9][CH:10]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[Cl:20])[C:11]([NH2:13])=[O:12].O.[OH-].[Na+]>ClCCCl>[S:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH2:7][CH2:8][NH:9][CH:10]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[Cl:20])[C:11]([NH2:13])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 21953219[2-(2-Thienyl)ethylamino](2-chlorophenyl)acetamide hydrochloride

생성물 1

HCID 9882604[2-(2-Thienyl)ethylamino](2-chlorophenyl)acetamide수율 88.2%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

24.8 g (0.075 mol) of [2-(2-thienyl)ethylamino](2-chlorophenyl)acetamide hydrochloride, prepared according to example 5 or 6, is mixed with 170 ml of water, then under mild cooling 30 ml of 10% sodium hydroxide solution and 170 ml of 1,2-dichloroethane are added. The phases are separated, the aqueous phase is extracted with 2×20 ml of 1,2-dichloroethane, the combined organic layer is evaporated in vacuo. Residue: 22 g, fast crystallizing oil. The raw product is recrystallized from 80 ml of isopropyl acetate to give 19.5 g of the crystalline base of formula (VII). Yield: 88.2%, mp.: 90-92° C.

후처리

  1. additionare added
  2. customThe phases are separated
  3. extractionthe aqueous phase is extracted with 2×20 ml of 1,2-dichloroethane
  4. customthe combined organic layer is evaporated in vacuo
  5. customResidue: 22 g, fast crystallizing oil
  6. customThe raw product is recrystallized from 80 ml of isopropyl acetate

출처 및 근거

ORD 기록
ord-ca0ba5bc6262407984d8102bdd6da567
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06180793B2

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