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Potassium Hydroxide → N-[3-{3-(piperidinomethyl)phenoxy}propyl]-2-mercaptoacetamide

HRID 1904324
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HRID 1904324 반응식
[N:1]1([CH2:7][C:8]2[CH:9]=[C:10]([CH:23]=[CH:24][CH:25]=2)[O:11][CH2:12][CH2:13][CH2:14][NH:15][C:16](=[O:22])[CH2:17][S:18]C(=O)C)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[OH-].[K+]>CO.O>[N:1]1([CH2:7][C:8]2[CH:9]=[C:10]([CH:23]=[CH:24][CH:25]=2)[O:11][CH2:12][CH2:13][CH2:14][NH:15][C:16](=[O:22])[CH2:17][SH:18])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
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참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 14625129HCID 14625129, 화합물

생성물 1

HCID 10663641N-[3-{3-(piperidinomethyl)phenoxy}propyl]-2-mercaptoacetamide

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

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온도
0 °C

실험 절차

2.23 g of this acetamide was dissolved in a mixed solvent of 30 ml of methanol and 3 ml of water, and cooled in an ice bath. 0.48 g of 85% potassium hydroxide was added to this solution, and stirred at 0° C. for 1.5 hours. pH of the reaction solution was adjusted to 7 by adding 2N aqueous hydrochloric acid, and extraction was carried out by adding 100 ml of dichloromethane and 50 ml of water. The dichloromethane layer was washed twice with water, and dried over anhydrous magnesium sulfate. The solvent was evapoated in vacuo to obtain the captioned colorless oily N-[3-{3-(piperidinomethyl)phenoxy}propyl]-2-mercaptoacetamide. Yield: 1.86 g.

후처리

  1. temperaturecooled in an ice bath
  2. additionby adding
  3. extraction2N aqueous hydrochloric acid, and extraction
  4. additionby adding 100 ml of dichloromethane and 50 ml of water
  5. washThe dichloromethane layer was washed twice with water
  6. dry with materialdried over anhydrous magnesium sulfate

출처 및 근거

ORD 기록
ord-700b68cf05334e948059c7de2139b87b
출처 데이터셋
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04837316

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