Dimethylformamide → AZ-2088

HRID 1657330ノート

反応式

HRID 1657330 の反応式
[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]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 123691-BromoheptaneHCID 21532766HCID 21532766、化合物

生成物 1

HCID 29942AZ-2088

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

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).

後処理

  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.)

出典と根拠

ORDレコード
ord-a1e4fbf499da4448b9e3bbfc581a6fc8
出典データセット
uspto-grants-1976_06
特許番号
US03960539

反応ノート

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