Dimethylformamide → HCID 178522035, 화합물

HRID 35027

반응식

HRID 35027 반응식
[F:1][C:2]([F:23])([C:16]([F:22])([F:21])[C:17]([F:20])([F:19])[F:18])[C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][CH2:13][C:14]#[N:15])=[CH:8][CH:7]=1)=[O:4].[N-:24]=[N+:25]=[N-:26].[Na+].[Cl-].[NH4+].CN(C)C=O>O>[F:1][C:2]([F:23])([C:16]([F:21])([F:22])[C:17]([F:19])([F:20])[F:18])[C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][CH2:13][C:14]2[NH:26][N:25]=[N:24][N:15]=2)=[CH:8][CH:7]=1)=[O:4]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 212977082,2,3,3,4,4,4-heptafluoro-N-[4-(2-cyanoethyl)phenyl]butanamide

생성물 1

HCID 178522035HCID 178522035, 화합물수율 43.3%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
130 °C

실험 절차

A mixture of 2,2,3,3,4,4,4-heptafluoro-N-[4-(2-cyanoethyl)phenyl]butanamide (3.9 g), sodium azide (3.7 g), ammonium chloride (3 g) and dimethylformamide (60 mL) was stirred under a nitrogen atmosphere and heated in a 130° C. oil bath for 48 hours. Water (300 mL) was added to the hot mixture to dissolve all suspended salts and the solution was allowed to cool to room temperature. More water was added and the precipitate was collected by filtration. The tan solid was dried at 65° C. in vacuo overnight and recrystallized from a hexane/tetrahydrofuran mixture to give 1.9 g (43% yield) of the title compound as a tan solid, m.p. 161°-162° C.

후처리

  1. dissolutionto dissolve all suspended salts
  2. temperatureto cool to room temperature
  3. filtrationthe precipitate was collected by filtration
  4. customThe tan solid was dried at 65° C. in vacuo overnight
  5. customrecrystallized from a hexane/tetrahydrofuran mixture

출처 및 근거

ORD 기록
ord-9153dc27639e4a4bb14481582c20460a
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764623

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