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Methanesulfonyl chloride → HCID 54083760, 화합물

HRID 342747
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HRID 342747 반응식
[CH3:1][C:2]([NH:8][C:9](=[O:18])[C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[C:12]([Cl:17])[CH:11]=1)([CH3:7])[C:3]([CH2:5][OH:6])=[O:4].C(N(C(C)C)CC)(C)C.[CH3:28][S:29](Cl)(=[O:31])=[O:30]>C(Cl)Cl>[CH3:7][C:2]([NH:8][C:9](=[O:18])[C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[C:12]([Cl:17])[CH:11]=1)([CH3:1])[C:3]([CH2:5][O:6][S:29]([CH3:28])(=[O:31])=[O:30])=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 54349857HCID 54349857, 화합물

생성물 1

HCID 54083760HCID 54083760, 화합물수율 63%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

N-(1',1'-dimethyl-3'-hydroxyacetonyl)-3,5-dichlorobenzamide (1.0 gm, 0.00345 m) was dissolved in methylene chloride (25 ml) and diisopropylethylamine (0.44 gm, 0.0035 m) and cooled to about 5° C. under a nitrogen atmosphere. While the solution was stirred magnetically, methanesulfonylchloride (0.475 gm, 0.0041 m) was added dropwise. After its addition, the mixture was stirred about an hour longer while maintaining the temperature at 5°-10° C. The mixture was then poured into ice water (500 ml) containing methylene chloride (100 ml). The organic layer was separated and was washed with cold 1% hydrochloric acid, saturated sodium bicarbonate, water and brine, and then dried over anhydrous potassium carbonate. The solvent was removed and 800 mg of the desired product was obtained.

후처리

  1. additionAfter its addition
  2. stirringthe mixture was stirred about an hour longer
  3. temperaturewhile maintaining the temperature at 5°-10° C
  4. customThe organic layer was separated
  5. washwas washed with cold 1% hydrochloric acid, saturated sodium bicarbonate, water and brine
  6. dry with materialdried over anhydrous potassium carbonate
  7. customThe solvent was removed

출처 및 근거

ORD 기록
ord-a2b066b84b704b32bc51d8721a2005ce
출처 데이터셋
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05859063

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