Water → HCID 67244725, 화합물

HRID 2425532노트

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HRID 2425532 반응식
[CH2:1]([N:8]([CH2:14]OC)[CH2:9][Si](C)(C)C)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:17]([O:20][C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=1/[CH:28]=[CH:29]/[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[Br:36])(=[O:19])[CH3:18].O>C1(C)C=CC=CC=1.FC(F)(F)C(O)=O>[C:17]([O:20][C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=1[C@H:28]1[C@H:29]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=2[Br:36])[CH2:9][N:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:14]1)(=[O:19])[CH3:18]

참가 물질

6

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HCID 962WaterHCID 353442Benzyl(methoxymethyl)((trimethylsilyl)methyl)amineHCID 44139027Phenol, 2-[(1E)-2-(2-bromophenyl)ethenyl]-4-chloro-, 1-acetate

생성물 1

HCID 67244725HCID 67244725, 화합물

시약·촉매·용매 2

HCID 6422Trifluoroacetic acid촉매HCID 1140Toluene용매

실험 절차

N-benzyl-N-methoxymethyl-N-(trimethylsilylmethyl)amine (5.0 g, 21.06 mmol) was added dropwise with a syringe over 30 minutes to a suspension of (E)-2-(2-bromostyryl)-4-chlorophenyl acetate (Example 1; 7.0 g, 19.9 mmol) in toluene (25 ml) containing trifluoroacetic acid (3 drops) while stirring at room temperature. After additional stirring for one hour water (10 ml) was added. The toluene layer was separated. The aqueous layer was extracted with toluene (25 ml). The combined organic layers were dried with Na2SO4 and evaporated under vacuum to give the crude cycloadduct as a clear and colorless oil, 10.76 g (>100%) in quantitative yield.

후처리

  1. additionwas added
  2. customThe toluene layer was separated
  3. extractionThe aqueous layer was extracted with toluene (25 ml)
  4. dry with materialThe combined organic layers were dried with Na2SO4
  5. customevaporated under vacuum
  6. customto give the crude cycloadduct as a clear and colorless oil, 10.76 g (>100%) in quantitative yield

출처 및 근거

ORD 기록
ord-e6441431342a4e2ab9d9546a6e317f4d
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07964739B2

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