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Hydrochloric Acid → HCID 22218673、化合物

HRID 1795673
ノート
印刷プレビュー

反応式

HRID 1795673 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

HCID 22218673HCID 22218673、化合物収率 80.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 1140
Toluene
溶媒
2 回

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-c92c128368cb45ca9fd938a11206964d
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07027327B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート