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Triethylamine → 3-Iodo-4-methylbenzonitrile

HRID 1619137
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HRID 1619137 반응식
FC(F)(F)C(OC(=O)C(F)(F)F)=O.[I:14][C:15]1[CH:16]=[C:17]([CH:21]=[CH:22][C:23]=1[CH3:24])[C:18]([NH2:20])=O.C(N(CC)CC)C.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[I:14][C:15]1[CH:16]=[C:17]([CH:21]=[CH:22][C:23]=1[CH3:24])[C:18]#[N:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 9845Trifluoroacetic anhydrideHCID 11430Potassium CarbonateHCID 8333293-Iodo-4-methylbenzamide

생성물 1

HCID 121296213-Iodo-4-methylbenzonitrile수율 80.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회
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실험 절차

2,2,2-trifluoroacetic anhydride (8.00 mL, 57.5 mmol) was added dropwise to a stirred solution of 3-iodo-4-methylbenzamide (preparation 48a, 6.00 g, 23.0 mmol) and triethylamine (8.10 mL, 57.5 mmol) in dichloromethane (50 mL) at 0° C. The mixture was warmed to room temperature and stirred for 2 hours. Further dichloromethane and saturated aqueous potassium carbonate solution were added and the organic layer was washed with 2M aqueous hydrochloric acid, 2M aqueous sodium hydroxide solution, brine, dried (MgSO4) and evaporated to give the title compound (4.50 g, 80%) as a pale orange solid.

후처리

  1. washthe organic layer was washed with 2M aqueous hydrochloric acid, 2M aqueous sodium hydroxide solution, brine
  2. dry with materialdried (MgSO4)
  3. customevaporated

출처 및 근거

ORD 기록
ord-bc79983383474776b1875e5879140fdf
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772288B2

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