Sodium Chloride → HCID 21901780, 화합물

HRID 719738노트

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HRID 719738 반응식
S(Cl)(C)(=O)=O.[N+:6]([C:9]1[CH:14]=[CH:13][C:12]([N:15]2[CH2:19][CH2:18][CH2:17][CH:16]2[CH2:20]O)=[CH:11][CH:10]=1)([O-:8])=[O:7].C(N(CC)CC)C.[Cl-:29].[Na+]>CN(C=O)C>[Cl:29][CH2:20][CH:16]1[CH2:17][CH2:18][CH2:19][N:15]1[C:12]1[CH:13]=[CH:14][C:9]([N+:6]([O-:8])=[O:7])=[CH:10][CH:11]=1

참가 물질

6

반응물 4

HCID 5234Sodium ChlorideHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 6056432-Pyrrolidinemethanol, 1-(4-nitrophenyl)-

생성물 1

HCID 21901780HCID 21901780, 화합물수율 882.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

27.9 ml (0.36 mol) of mesyl chloride were added dropwise to a solution of [1-(4-nitrophenyl)pyrrolidin-2-yl]methanol (66.7 g, 0.03 mol), 300 ml of anhydrous DMF and 58.5 ml (0.42 mol) of anhydrous triethylamine, cooled in an ice bath. The temperature was allowed to rise to 20° C. over one hour with stirring. 35.2 g (0.6 mol) of sodium chloride were added and the mixture was heated at 100° C. for one hour. The reaction medium was poured into 1.4 l of ice-water. The precipitate was filtered off, washed with water, dried and recrystallized from isopropanol. 63.7 g of a yellow powder (1) were thus obtained.

후처리

  1. temperaturecooled in an ice bath
  2. filtrationThe precipitate was filtered off
  3. washwashed with water
  4. customdried
  5. customrecrystallized from isopropanol

출처 및 근거

ORD 기록
ord-db83a59d84f545d3a4a2b3b805ca0889
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07132543B2

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