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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → 2,2-Dichloro-N-[(2-ethoxyethoxy)methyl]-N-(3-methylbutyl)acetamide

HRID 1905559
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HRID 1905559 반응식
[CH2:1]([N:6]([CH2:12]Cl)[C:7](=[O:11])[CH:8]([Cl:10])[Cl:9])[CH2:2][CH:3]([CH3:5])[CH3:4].[CH2:14]([O:16][CH2:17][CH2:18][OH:19])[CH3:15].C(N(CC)CC)C.O>C1C=CC=CC=1>[CH2:1]([N:6]([CH2:12][O:19][CH2:18][CH2:17][O:16][CH2:14][CH3:15])[C:7](=[O:11])[CH:8]([Cl:10])[Cl:9])[CH2:2][CH:3]([CH3:5])[CH3:4]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8076Glycol monoethyl etherHCID 8471TriethylamineHCID 200358492,2-Dichloro-N-(chloromethyl)-N-(3-methylbutyl)acetamide

생성물 1

HCID 138242942,2-Dichloro-N-[(2-ethoxyethoxy)methyl]-N-(3-methylbutyl)acetamide

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

The solution of N-isopentyl-N-chloromethyldichloroacetamide (24.7 g., 0.1 mole) and 2-ethoxyethanol (9.9 g., 10.7 ml., 0.11 mole) in dry benzene (70 ml) is weighed in a four-necked, round-bottom flask of 250 ml, equipped with a calcium chloride tube, reflux condenser, mechanical stirrer, dropping funnel and thermometer. Triethylamine (10.1 g., 13.9 ml., 0.1 mole) is added to this solution under stirring and cooling by water in such a rate that the temperature is maintained below 40° C. After the addition is complete, the mixture is stirred for an additional 2 hours at room temperature. The mixture is washed with water (2×100 ml.) to remove triethylamine hydrochloride and the possible hydrophilic side-product, the benzene solution is dried over anhydrous sodium sulfate after distillation of the solvent and the residue is evaporated to dry under reduced pressure to give 27.9 g. (93%) of the named product as a pale yellow oil which is of 96% purity according to analysis by gas chromatography and is directly useful for practical purposes without any purification; nD25 =1.4649.

후처리

  1. customequipped with a calcium chloride tube
  2. temperaturereflux condenser, mechanical stirrer
  3. temperatureis maintained below 40° C
  4. additionAfter the addition
  5. stirringthe mixture is stirred for an additional 2 hours at room temperature
  6. washThe mixture is washed with water (2×100 ml.)
  7. customto remove triethylamine hydrochloride
  8. dry with materialthe possible hydrophilic side-product, the benzene solution is dried over anhydrous sodium sulfate
  9. distillationafter distillation of the solvent
  10. customthe residue is evaporated
  11. customto dry under reduced pressure
  12. customto give 27.9 g
  13. customis directly useful for practical purposes without any purification

출처 및 근거

ORD 기록
ord-ffab82cca99e478cae89e2ba99898984
출처 데이터셋
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04843177

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