Sodium Hydroxide → [(4-Chloro-1H-pyrazol-1-yl)oxy]methyl thiocyanate

HRID 34952

반응식

HRID 34952 반응식
[OH-].[Na+].[Cl:3][C:4]1[CH:5]=[N:6][N:7]([OH:9])[CH:8]=1.Cl[CH2:11][S:12][C:13]#[N:14].[OH-].C([N+](CCCC)(CCCC)CCCC)CCC>C(Cl)Cl>[Cl:3][C:4]1[CH:5]=[N:6][N:7]([O:9][CH2:11][S:12][C:13]#[N:14])[CH:8]=1

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 76755Thiocyanic acid, chloromethyl esterHCID 2723671Tetrabutylammonium HydroxideHCID 133912524-Chloro-1H-pyrazol-1-ol

생성물 1

HCID 14011041[(4-Chloro-1H-pyrazol-1-yl)oxy]methyl thiocyanate수율 71.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

50 ml of a 5% strength aqueous sodium hydroxide solution were added to 5 g (42 mMol) of 4-chloro-1-hydroxypyrazole, 13.5 g (126 mMol) of chloromethyl thiocyanate and 50 ml of methylene chloride. After the addition of 1 g (4 mMol) of tetra-n-butylammonium hydroxide, the mixture was stirred at room temperature for 24 hours. Thereafter, the organic phase was separated off, dried and evaporated down. Distillation of the residue under reduced pressure (airbath at 140° C./3 mbar) gave 5.7 g (71% of theory) of 4-chloro-1-[(thiocyanato)-methoxy]-pyrazole (compound No. 1), which was recrystallized from ether/petroleum ether (mp. 60° C.).

후처리

  1. customThereafter, the organic phase was separated off
  2. customdried
  3. customevaporated down
  4. distillationDistillation of the residue under reduced pressure (airbath at 140° C./3 mbar)

출처 및 근거

ORD 기록
ord-e1f2e11ee6ab46f19657e1637b95bd26
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764527

연결된 노트

불러오는 중…