6-Dimethylaminohexan-1-ol → Ammonium Hydroxide

HRID 621765

反応式

HRID 621765 の反応式
[CH2:1]([N:13]=[C:14]=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[CH3:16][N:17]([CH3:25])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][OH:24]>O1CCCC1>[NH4+:13].[OH-:15].[CH3:16][N:17]([CH3:25])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][O:24][C:14](=[O:15])[NH:13][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

参加物

5

反応物 2

HCID 746236-Dimethylaminohexan-1-olHCID 77873Dodecane, 1-isocyanato-

生成物 2

HCID 14923Ammonium HydroxideHCID 14407596Dodecylcarbamic acid 6-(dimethylamino)hexyl ester

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1.1 gm (5 meq) of dodecyl isocyanate and 726 mg (5 meq) of 6-(dimethylamino)hexanol are combined in 5 ml of tetrahydrofuran and reacted over weekend at room temperature. The insoluble crystals are filtered, washed with ethyl acetate and the filtrate and washings combined, evaporated under reduced pressure (<30° C.) and dried in vacuo. The product is purified by silica gel chromatography in the system CH2Cl2 :CH3OH:NH4OH (65:25:4). Fractions 34-46 are combined, evaporated and dried in vacuo to yield 300 mg (Rf 0.9 S.G. CH2Cl2, CH3OH, NH4OH) of title compound.

後処理

  1. customreacted over weekend at room temperature
  2. filtrationThe insoluble crystals are filtered
  3. washwashed with ethyl acetate
  4. customevaporated under reduced pressure (<30° C.)
  5. customdried in vacuo
  6. customThe product is purified by silica gel chromatography in the system CH2Cl2 :CH3OH:NH4OH (65:25:4)
  7. customevaporated
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-10fe8ebfd8054af49d4995ba11d7035c
出典データセット
uspto-grants-1989_04
特許番号
US04824996

関連ノート

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