Triethylamine → HCID 19854909, 화합물

HRID 1194006노트

반응식

HRID 1194006 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[C:14]([Cl:15])=[CH:13][C:12]([Cl:16])=[CH:11][N:10]=2)[CH:5]=[C:4]([CH3:17])[C:3]=1[NH:18][C:19]([NH:21][C:22]([CH3:25])([CH3:24])[CH3:23])=S.[I-].ClC1C=CC=C[N+]=1C.C(N(CC)CC)C>C(#N)C>[CH3:17][C:4]1[CH:5]=[C:6]([O:8][C:9]2[C:14]([Cl:15])=[CH:13][C:12]([Cl:16])=[CH:11][N:10]=2)[CH:7]=[C:2]([CH3:1])[C:3]=1[N:18]=[C:19]=[N:21][C:22]([CH3:25])([CH3:24])[CH3:23]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 1670692-Chloro-1-methylpyridinium iodideHCID 19854910HCID 19854910, 화합물

생성물 1

HCID 19854909HCID 19854909, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

A reaction vessel is charged with 16.6 g of N-[2,6-dimethyl-4-(3,5-dichloro-2-pyridyloxy)phenyl]-N'-tert-butylthiourea and 12.8 g of 2-chloro-1-methylpyridinium iodide in 150 ml of acetonitrile. With stirring, a solution of 8.4 g of triethylamine in 80 ml of acetonitrile is added dropwise at room temperature. The reaction mixture is subsequently stirred for 2 hours at 80° C. and then concetrated by rotary evaporation at 50° C. 150 ml of hexane are added to the residue and the resultant solution is filtered. The hexane phase is washed with three 30 ml portions of cold water, dried over sodium sulfate and filtered. The filtrate is concentrated by evaporation, affording the title compound of the formula ##STR5## as a clear pale yellow oil which crystallises on standing and has a melting point of 69°-71° C. (compound 1).

후처리

  1. stirringThe reaction mixture is subsequently stirred for 2 hours at 80° C.
  2. customconcetrated by rotary evaporation at 50° C
  3. addition150 ml of hexane are added to the residue
  4. filtrationthe resultant solution is filtered
  5. washThe hexane phase is washed with three 30 ml portions of cold water
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate is concentrated by evaporation

출처 및 근거

ORD 기록
ord-4265b2fe70054b829e02efa18a6e545a
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04812466

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