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2-(Dimethylamino)ethanol → HCID 53923166, 화합물

HRID 2225707
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HRID 2225707 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[O:11][CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([C:21](=[O:25])[C:22]([OH:24])=[O:23])=[CH:17][CH:16]=1.[CH3:26][N:27]([CH3:31])[CH2:28][CH2:29]O>ClCCl>[CH3:26][N:27]([CH3:31])[CH2:28][CH2:29][O:23][C:22](=[O:24])[C:21](=[O:25])[C:18]1[CH:19]=[CH:20][C:15]([O:14][CH2:13][CH2:12][O:11][C:2]2[CH:3]=[CH:4][C:5]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[CH:1]=2)=[CH:16][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 79022-(Dimethylamino)ethanolHCID 19004267HCID 19004267, 화합물

생성물 1

HCID 53923166HCID 53923166, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

The acid chloride, prepared from 4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alphaoxobenzeneacetic acid (0.5 g) as described in Example 6, was dissolved in dichloromethane (10 mL) and added dropwise to a stirred, cold (<-50° C.) mixture of 2-(dimethylamino)ethanol (0.178 g) in dichloromethane (10 mL). The cooling bath was removed and the mixture stirred for 1 hour at room temperature. The mixture was diluted with dichloromethane and washed once with saturated aqueous sodium bicarbonate, once with water, and the organic solution was dried (Na2SO4), filtered, and evaporated to give crude product. Crystallization from diethyl ether-hexane provided pure 4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alpha-oxobenzeneacetic acid 2-(dimethylamino)ethyl ester as a colorless solid, mp 93°-94° C.

후처리

  1. customThe cooling bath was removed
  2. additionThe mixture was diluted with dichloromethane
  3. washwashed once with saturated aqueous sodium bicarbonate, once with water
  4. dry with materialthe organic solution was dried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated
  7. customto give crude product
  8. customCrystallization from diethyl ether-hexane provided pure 4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alpha-oxobenzeneacetic acid 2-(dimethylamino)ethyl ester as a colorless solid, mp 93°-94° C.

출처 및 근거

ORD 기록
ord-d3b91e4f16c441a4aac0ff0ca67f80f2
출처 데이터셋
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05344843

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