Water → HCID 178418853, 화합물

HRID 10517

반응식

HRID 10517 반응식
[C:1]([O:5][C:6]([NH:8][C@H:9]1[CH2:14][CH2:13][C@H:12](OS(C)(=O)=O)[CH2:11][CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C[Si]([N:24]=[N+:25]=[N-:26])(C)C.[F-].[Cs+].O>CN(C)C=O>[C:1]([O:5][C:6]([NH:8][C@@H:9]1[CH2:14][CH2:13][C@H:12]([N:24]=[N+:25]=[N-:26])[CH2:11][CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 25953Cesium fluorideHCID 78378AzidotrimethylsilaneHCID 178418975HCID 178418975, 화합물

생성물 1

HCID 178418853HCID 178418853, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of Intermediate 36 (196 g) and trimethylsilyl azide (283 ml, Tokyo Kasei Kogyo) in dimethylformamide (667 ml) was added with cesium fluoride (305 g, Wako Pure Chemical Industries) with stirring and stirred at 70° C. for 4 days. The reaction mixture was cooled to room temperature and then added twice with water in a volume of 2.75 l in total. This reaction mixture was stirred with ice cooling for 2 hours, and the deposited precipitates were collected by filtration. Then, the precipitates were washed with water to obtain a roughly purified product of the title compound (142 g).

후처리

  1. stirringstirred at 70° C. for 4 days
  2. stirringThis reaction mixture was stirred with ice cooling for 2 hours
  3. customthe deposited precipitates
  4. filtrationwere collected by filtration
  5. washThen, the precipitates were washed with water

출처 및 근거

ORD 기록
ord-b811f8e37f91454ca9c82dfe2654d854
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094789B2

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