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Dichloromethane → HCID 19875836, 화합물

HRID 1886345
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HRID 1886345 반응식
O[CH:2]([C:6]1[CH:11]=[CH:10][C:9]([NH:12][C:13](=[O:15])[CH3:14])=[C:8]([N+:16]([O-:18])=[O:17])[CH:7]=1)[CH:3]([CH3:5])[CH3:4].[Cl:19]CCl.CS(Cl)(=O)=O.C(=O)([O-])[O-].[Na+].[Na+]>O.C(N(CC)CC)C>[Cl:19][CH:2]([C:6]1[CH:11]=[CH:10][C:9]([NH:12][C:13](=[O:15])[CH3:14])=[C:8]([N+:16]([O-:18])=[O:17])[CH:7]=1)[CH:3]([CH3:5])[CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 10340Sodium CarbonateHCID 31297Methanesulfonyl chlorideHCID 19875845HCID 19875845, 화합물

생성물 1

HCID 19875836HCID 19875836, 화합물수율 100%

시약·촉매·용매 2

HCID 962Water용매
HCID 8471
Triethylamine
용매

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온도
0 °C

실험 절차

To a stirred solution of 36 parts of intermediate 15, namely N-[4-(1-hydroxy-2-methylpropyl)-2-nitrophenyl]acetamide and 390 parts of dichloromethane were added 35.0 parts of N,N-diethylethanamine. After cooling to 0° C., 20.0 parts of methanesulfonyl chloride were added dropwise to the previous mixture. Upon completion, stirring was continued for 12 hours at room temperature. The whole was poured into water and sodium carbonate was added while stirring. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated, yielding 39 parts (100%) of N-[4-(1-chloro-2-methylpropyl)-2-nitrophenyl]acetamide (interm. 16).

후처리

  1. additionwas added
  2. stirringwhile stirring
  3. extractionThe product was extracted with dichloromethane
  4. customThe extract was dried
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-9094aa29297946088d0876be37701e8a
출처 데이터셋
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05151421

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