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2-Methylbenzenesulfonic acid → HCID 20551711, 화합물

HRID 1446957
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HRID 1446957 반응식
[CH3:1][O:2][CH:3]([O:10][CH3:11])[CH2:4][NH:5][C:6](=[O:9])[CH2:7][Cl:8].[CH2:12](O)CCO.C1(C)C(S(O)(=O)=O)=CC=CC=1>C(OCC)C>[O:10]1[CH2:11][CH2:12][CH2:1][O:2][CH:3]1[CH2:4][NH:5][C:6](=[O:9])[CH2:7][Cl:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 69252-Methylbenzenesulfonic acidHCID 104421,3-PropanediolHCID 193700222-Chloro-N-(2,2-dimethoxyethyl)acetamide

생성물 1

HCID 20551711HCID 20551711, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
120 °C

실험 절차

N-(2,2-Dimethoxyethyl)-2-chloroacetamide (18.2 grams; 0.1 mole), 1,3-propanediol (7.61 grams; 0.1 mole) and 10 drops of a solution of 1 gram of toluenesulfonic acid in 100 ml of diethyl ether were charged into a glass reaction vessel fitted with a mechanical stirrer, thermometer, distillation head and condenser. The mixture was stirred and heated at about 120° C. for a period of about 1 hour while byproduct methanol was distilled off. The mixture was cooled to room temperature, sodium carbonate (2 grams) was added, and the slurry stirred for a period of about 1 hour. The slurry was filtered and the filtrate was stripped of solvent by mild warming under reduced pressure to yield the desired product N-(1,3-dioxan-2-ylmethyl)-2-chloracetamide as a residue.

후처리

  1. customfitted with a mechanical stirrer
  2. distillationthermometer, distillation head and condenser
  3. distillationwas distilled off
  4. temperatureThe mixture was cooled to room temperature
  5. additionsodium carbonate (2 grams) was added
  6. stirringthe slurry stirred for a period of about 1 hour
  7. filtrationThe slurry was filtered
  8. temperatureby mild warming under reduced pressure

출처 및 근거

ORD 기록
ord-4a4dd4ba6c164ea1a20c12111b79d810
출처 데이터셋
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04314840

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