Octadecylamine → N-octadecyl-o-iodobenzamide

HRID 1277909

반응식

HRID 1277909 반응식
[CH2:1]([NH2:19])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].[I:20][C:21]1[CH:29]=[CH:28][CH:27]=[CH:26][C:22]=1[C:23](Cl)=[O:24].Cl.C(N)CCCCCCCCCCCCCCCCC>CCOCC.C(O)C>[CH2:1]([NH:19][C:23](=[O:24])[C:22]1[CH:26]=[CH:27][CH:28]=[CH:29][C:21]=1[I:20])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

참가 물질

6

반응물 3

HCID 15793OctadecylamineHCID 691122-Iodobenzoyl chlorideHCID 519552Stearamine hydrochloride

생성물 1

HCID 13020107N-octadecyl-o-iodobenzamide수율 8%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매2회

실험 절차

A solution of 17.9 g of octadecylamine in a mixture of 300 ml of ether and 10 ml of ethanol was reacted with a solution of 8.0 g of o-iodobenzoyl chloride in 25 ml of ether for 10 minutes. The precipitate which formed contained octadecylamine hydrochloride. This precipitate was recovered and discarded. The volume was thereafter reduced to approximately half at 65° on a water bath. The resulting precipitate was recovered in accordance with the procedure of Example 3. The crude product was recrystallized from benzene to yield 1.2 g of N-octadecyl-o-iodobenzamide as a white microcrystalline solid, m.p. 94°-96°, Rf 0.77.

후처리

  1. customThe precipitate which formed
  2. customThis precipitate was recovered
  3. customThe volume was thereafter reduced to approximately half at 65° on a water bath
  4. customThe resulting precipitate was recovered in accordance with the procedure of Example 3
  5. customThe crude product was recrystallized from benzene

출처 및 근거

ORD 기록
ord-47dc18bce46f4196a740298cca09af88
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04279887

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