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Hydrochloric Acid → HCID 22218673, 화합물

HRID 1795673
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HRID 1795673 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][N:8]1[CH:12]=[CH:11][CH:10]=[CH:9]1.N1C=CC=CC=1.[C:19](Cl)(=[O:30])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH:28]=[CH2:29].Cl>O.C1(C)C=CC=CC=1>[C:19]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][N:8]1[CH:9]=[CH:10][CH:11]=[CH:12]1)(=[O:30])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH:28]=[CH2:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 3804210-Undecenoyl chlorideHCID 134196986-(1H-Pyrrol-1-yl)hexan-1-ol

생성물 1

HCID 22218673HCID 22218673, 화합물수율 80.5%

시약·촉매·용매 2

HCID 962Water용매
HCID 1140
Toluene
용매
2회

실험 절차

62.0 g (0.371 mol) of N-(6-hydroxyhexyl)-pyrrole, 33.2 g (0.420 mol) of dry pyridine, and 1850 ml of dry toluene were put in a 2-liter reactor, and 300 ml of a dry toluene solution of 75.7 g (0.373 mol) of 10-undecenoylchloride was dropped thereto at 20° C. or below. The dropping time was 30 minutes. Thereafter, the mixture was stirred at the same temperature for one hour. The reaction mixture was poured into 1.5 liter of iced water, and was made acidic with use of 1N hydrochloric acid. It was subjected to ethyl acetate extraction, an organic layer was washed with water and concentrated brine and was dried using anhydrous magnesium sulfate, and the solvent was removed. As a result, 128.2 g of crude substance was obtained. This was subjected to purification by silicagel column with use of n-hexane/acetone=20/1, whereby 99.6 g of N-[6-(10-undecenoyloxy)hexyl]-pyrrole was obtained. The yield was 80.1%. The reaction of the step 4 is expressed by a reaction formula (15) shown below:

후처리

  1. customat 20° C. or below
  2. extractionIt was subjected to ethyl acetate extraction
  3. washan organic layer was washed with water and concentrated brine
  4. customwas dried
  5. customthe solvent was removed
  6. customAs a result, 128.2 g of crude substance was obtained
  7. customThis was subjected to purification by silicagel column with use of n-hexane/acetone=20/1

출처 및 근거

ORD 기록
ord-c92c128368cb45ca9fd938a11206964d
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07027327B2

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