Water → HCID 178444465, 화합물

HRID 2254994노트

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HRID 2254994 반응식
[CH2:1]([C@H:6]1[CH2:11][CH2:10][C@H:9]([CH2:12][CH2:13][CH2:14][O:15][C:16]2[CH:23]=[CH:22][C:19]([CH:20]=[O:21])=[CH:18][CH:17]=2)[CH2:8][CH2:7]1)[CH2:2][CH2:3][CH2:4][CH3:5].[CH2:24]([CH:29]([CH2:32]O)[CH2:30][OH:31])[CH2:25][CH2:26][CH2:27][CH3:28].S(=O)(=O)(O)O.O>C1(C)C=CC=CC=1>[CH2:24]([C@@H:29]1[CH2:30][O:31][C@@H:20]([C:19]2[CH:18]=[CH:17][C:16]([O:15][CH2:14][CH2:13][CH2:12][C@H:9]3[CH2:10][CH2:11][C@H:6]([CH2:1][CH2:2][CH2:3][CH2:4][CH3:5])[CH2:7][CH2:8]3)=[CH:23][CH:22]=2)[O:21][CH2:32]1)[CH2:25][CH2:26][CH2:27][CH3:28]

참가 물질

6

반응물 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 1175092-Pentyl-1,3-propanediolHCID 178444467HCID 178444467, 화합물

생성물 1

HCID 178444465HCID 178444465, 화합물수율 20.3%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 2.1 g of 4-[3-(trans-4-pentylcyclohexyl)-1-propyloxy]benzaldehyde and 1.2 g of 2-pentyl-1,3-propanediol in 50 ml of toluene was treated with 2 drops of 10% (vol., sulfuric acid. The mixture was heated to boiling for 2.5 hours, with the resulting water being distilled off simultaneously. Then, 4 drops of triethylamine were added to the reaction mixture. After cooling the mixture was washed with 20 ml of 1N sodium hydrogen carbonate solution and twice with 20 ml of water each time, dried over sodium sulfate, filtered and concentrated. Chromatography of the residue on silica gel with toluene gave 0.6 g of trans-5-pentyl-2-(4-[3-(trans-4-pentylcyciohexyl)-1-propyloxy]phenyl)-1,3-dioxane. M.p. (C-SB) 65° C. transition SB -N 73° C., cl.p (N-I) 128° C.

후처리

  1. temperatureThe mixture was heated
  2. distillationdistilled off simultaneously
  3. additionThen, 4 drops of triethylamine were added to the reaction mixture
  4. temperatureAfter cooling the mixture
  5. washwas washed with 20 ml of 1N sodium hydrogen carbonate solution and twice with 20 ml of water each time
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-92c44f29258640bda3d104c98171bdba
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05238600

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