6-Dimethylaminohexan-1-ol → Ammonium Hydroxide

HRID 621765

반응식

HRID 621765 반응식
[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]

참가 물질

5

반응물 2

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

생성물 2

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-10fe8ebfd8054af49d4995ba11d7035c
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824996

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