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Ethylene Glycol → HCID 20551713, 화합물

HRID 1446956
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HRID 1446956 반응식
[CH3:1][O:2][CH:3]([O:10][CH3:11])[CH2:4][NH:5][C:6](=[O:9])[CH2:7][Cl:8].C(O)CO.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(OCC)C>[O:10]1[CH2:11][CH2:1][O:2][CH:3]1[CH2:4][NH:5][C:6](=[O:9])[CH2:7][Cl:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 193700222-Chloro-N-(2,2-dimethoxyethyl)acetamide

생성물 1

HCID 20551713HCID 20551713, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

N-(2,2-Dimethoxyethyl)-2-chloroacetamide (18.1 grams; 0.10 mole) ethylene glycol (6.82 grams; 0.11 mole) and 10 drops of a solution of one gram of p-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 to about 95° C. to 100° C. Byproduct methanol was distilled off. When no further methanol was evolved, the mixture was cooled to room temperature, sodium carbonate (2 grams) was added and the slurry was stirred for a period of about 1 hour. The slurry was then filtered and the filtrate fractionally distilled under reduced pressure the desired product N-(1,3-dioxolan-2-ylmethyl)-2-chloroacetamide was obtained as a fraction boiling at 109° C.-110° C. at 0.15 mm Hg which, when cooled, solidfied. The solid had a melting point of 61° C.-63° C.

후처리

  1. customfitted with a mechanical stirrer
  2. distillationthermometer, distillation head and condenser
  3. temperatureheated to about 95° C. to 100° C
  4. distillationByproduct methanol was distilled off
  5. additionsodium carbonate (2 grams) was added
  6. stirringthe slurry was stirred for a period of about 1 hour
  7. filtrationThe slurry was then filtered
  8. distillationthe filtrate fractionally distilled under reduced pressure the desired product N-(1,3-dioxolan-2-ylmethyl)-2-chloroacetamide
  9. customwas obtained as a fraction boiling at 109° C.-110° C. at 0.15 mm Hg which, when
  10. temperaturecooled

출처 및 근거

ORD 기록
ord-d2cf2094e96942c79660a51f111ae747
출처 데이터셋
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04314840

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