Triethylamine → HCID 14624341, 화합물

HRID 1650764

반응식

HRID 1650764 반응식
[N+:1]([C:4]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:6][C:5]=1[NH:14][N:15]=[C:16](Br)[C:17]([CH3:20])([CH3:19])[CH3:18])([O-:3])=[O:2].[CH2:22]([N:24]([CH2:27][CH3:28])[C:25]#[N:26])[CH3:23].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH2:22]([N:24]([C:25]1[N:14]([C:5]2[CH:6]=[CH:7][C:8]([C:10]([F:13])([F:12])[F:11])=[CH:9][C:4]=2[N+:1]([O-:3])=[O:2])[N:15]=[C:16]([C:17]([CH3:20])([CH3:19])[CH3:18])[N:26]=1)[CH2:27][CH3:28])[CH3:23]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12050DiethylcyanamideHCID 86743922HCID 86743922, 화합물

생성물 1

HCID 14624341HCID 14624341, 화합물수율 84.4%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

7.4 g (0.02 mol) of 2,2-dimethylpropionyl bromide 2-nitro-4-trifluoromethylphenylhydrazone and 2.0 g (0.02 mol) of N,N-diethylcyanamide were added to 100 ml of toluene. Then, 2.2 g (0.022 mol) of triethylamine was dropwise added under stirring at room temperature. After completion of the dropwise addition, stirring was continued at room temperature for further 1 hour. Then, 100 ml of toluene was added and washed with water. The organic layer was dried, and the solvent was distilled off. The residue was purified by silica gel column chromatography to obtain 6.5 g (yield: 84.4%) of the desired compound as a pale yellow liquid. Refractive index nD20 : 1.4911.

후처리

  1. additionAfter completion of the dropwise addition
  2. stirringstirring
  3. washwashed with water
  4. customThe organic layer was dried
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-4eb6eb4f9ae149d9bf2610c10b131d30
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04925864

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