Triethylamine → HCID 68872277, 화합물

HRID 2112038노트

반응식

HRID 2112038 반응식
[CH2:1]([NH:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].C(N(CC)CC)C.[Br:22][CH2:23][C:24](Cl)=[O:25]>C(Cl)Cl>[CH2:8]([N:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[C:24](=[O:25])[CH2:23][Br:22])[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 89602Bromoacetyl chlorideHCID 485395Benzenemethanamine, N-hexyl-

생성물 1

HCID 68872277HCID 68872277, 화합물수율 58.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

N-hexylbenzylamine (4.2 g, 21.953 mmol) and triethylamine (3.98 ml, 28.539 mmol) were mixed in DCM (20 ml) and cooled in an ice-bath. Bromacetyl chloride (3.455 mg, 21.953 mmol) in DCM (5 ml) was added. The mixture was stirred over weekend and the temperature was allowed going up to room temperature. The mixture was washed with water mixed with 1% hydrochloric acid (water phase pH˜4-5) and brine, dried with magnesium sulphate, and evaporated. Column chromatography of the residue on silica gel using ethyl acetate/heptane (10:90, then 20:80) as eluant gave 4.0 g desired product, yield 58%.

후처리

  1. temperaturecooled in an ice-bath
  2. customwas allowed going up to room temperature
  3. washThe mixture was washed with water
  4. additionmixed with 1% hydrochloric acid (water phase pH˜4-5) and brine
  5. dry with materialdried with magnesium sulphate
  6. customevaporated

출처 및 근거

ORD 기록
ord-4a770f917d7d410eaca8f49ddbd503ae
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07521461B2

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