Dimethylformamide → AZ-2088

HRID 1657330노트

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HRID 1657330 반응식
[CH3:1][N:2]([CH3:14])[CH:3]1[CH2:8][CH:7]([CH:9]([CH3:11])[CH3:10])[CH2:6][CH2:5][C:4]1([OH:13])[CH3:12].[CH2:15]([Br:22])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]C.[CH3:23]N(C)C=O>O>[Br-:22].[CH3:14][N+:2]([CH3:23])([CH2:1][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])[CH:3]1[CH2:8][CH:7]([CH:9]([CH3:11])[CH3:10])[CH2:6][CH2:5][C:4]1([OH:13])[CH3:12]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 123691-BromoheptaneHCID 21532766HCID 21532766, 화합물

생성물 1

HCID 29942AZ-2088

시약·촉매·용매 1

HCID 962Water용매

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온도
90 °C

실험 절차

Five grams of 2-dimethylamino-1-p-menthanol and 10 g. of heptyl bromide were dissolved in 5 ml. of dimethylformamide. The solution was warmed at 90°C (under nitrogen) for 16 hours, cooled to room temperature and diluted with water (approximately 100 ml.). The mixture was transferred to a separatory funnel and washed three times with ethyl ether (20-25 ml.). The neutral, aqueous phase was concentrated to dryness on a film evaporator (at 50°C). Ninety-five percent ethanol was added to the flask contents to assist the azeotropic removal of water. Last traces of DMF were removed at high vacuum (1 mm.). Yield of dimethyl heptyl (1-hydroxy-p-menthan-2-yl) ammonium bromide was 10.2 g. (100T of theory).

후처리

  1. temperaturecooled to room temperature
  2. customThe mixture was transferred to a separatory funnel
  3. washwashed three times with ethyl ether (20-25 ml.)
  4. concentrationThe neutral, aqueous phase was concentrated to dryness on a film evaporator (at 50°C)
  5. additionNinety-five percent ethanol was added to the flask contents
  6. customthe azeotropic removal of water
  7. customLast traces of DMF were removed at high vacuum (1 mm.)

출처 및 근거

ORD 기록
ord-a1e4fbf499da4448b9e3bbfc581a6fc8
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03960539

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