Acetic Acid → Dehydroabietylamine acetate

HRID 342733노트

반응식

HRID 342733 반응식
[CH3:1][CH:2]([C:4]1[CH:9]=[CH:8][C:7]2[C@:10]3([CH3:21])[C@@H:15]([CH2:16][CH2:17][C:6]=2[CH:5]=1)[C@@:14]([CH2:19][NH2:20])([CH3:18])[CH2:13][CH2:12][CH2:11]3)[CH3:3].[C:22]([OH:25])(=[O:24])[CH3:23]>C1(C)C=CC=CC=1>[CH3:3][CH:2]([C:4]1[CH:9]=[CH:8][C:7]2[C@:10]3([CH3:21])[C@@H:15]([CH2:16][CH2:17][C:6]=2[CH:5]=1)[C@@:14]([CH2:19][NH2:20])([CH3:18])[CH2:13][CH2:12][CH2:11]3)[CH3:1].[CH3:23][C:22]([OH:25])=[O:24]

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 62034Dehydroabietylamine

생성물 1

HCID 62418Dehydroabietylamine acetate수율 78%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

A solution of dehydroabietylamine (60%, 100 g, 0.21 mol) in toluene (170 mL) was treated with a second solution of glacial acetic acid (24 mL) in toluene (55 mL) at room temperature. The mixture was stored at room temperature overnight. The crystalline salt was collected by filtration, washed with cold toluene and recrystallized from boiling toluene (152 mL). The crystals were collected by filtration, washed with n-pentane and air-dried to give dehydroabietylamine acetate (47 g, 78%) as a white crystalline solid.

후처리

  1. filtrationThe crystalline salt was collected by filtration
  2. washwashed with cold toluene
  3. customrecrystallized
  4. filtrationThe crystals were collected by filtration
  5. washwashed with n-pentane
  6. customair-dried

출처 및 근거

ORD 기록
ord-120e4094533841d3b3446ac83d5b126b
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05859047

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