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Dimethyl Sulfoxide → HCID 44602516, 화합물

HRID 448540
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HRID 448540 반응식
C(Cl)(=O)C(Cl)=O.CS(C)=O.[Cl:11][CH2:12][CH2:13][C:14]1[C:19](=[O:20])[N:18]2[CH2:21][CH2:22][CH2:23][CH:24]([OH:25])[C:17]2=[N:16][C:15]=1[CH3:26].C(N(CC)CC)C>ClCCl>[Cl:11][CH2:12][CH2:13][C:14]1[C:19](=[O:20])[N:18]2[CH2:21][CH2:22][CH2:23][C:24](=[O:25])[C:17]2=[N:16][C:15]=1[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 155471943-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

생성물 1

HCID 44602516HCID 44602516, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매
3회

실험 절차

A solution of oxalylchloride (8.8 ml) in dichloromethane (20 ml) was cooled to −65° C. and a solution of dimethyl sulfoxide (6.5 ml) dissolved in dichloromethane (20 ml) was added to it slowly and stirred for 30 min. keeping the temperature at −65° C. a solution of 3-(2-chloroethyl)-9-hydroxy-2-methyl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-4-one (5 grams) (formula-7) dissolved in dichloromethane (30 ml) was added to it very slowly and stirred for 40 min. Triethyl amine was added to the reaction mixture and then quenched with water. The organic layer was separated, washed with aqueous sodium carbonate and water. The solvent from the organic layer was distilled off under reduced pressure to provide the title compound.

후처리

  1. additionwas added to it slowly
  2. customat −65° C.
  3. additionwas added to it very slowly
  4. stirringstirred for 40 min
  5. customquenched with water
  6. customThe organic layer was separated
  7. washwashed with aqueous sodium carbonate and water
  8. distillationThe solvent from the organic layer was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-0768b6b37ae74e278e21280929a41dd7
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481729B2

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