Water → HCID 14257790、化合物

HRID 868433ノート

反応式

HRID 868433 の反応式
I[CH2:2][CH:3]1[CH2:12][CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4]1.[OH:13][CH:14]([C:20]1[CH:21]=[C:22]([OH:26])[CH:23]=[CH:24][CH:25]=1)[CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].[OH-].[Na+].O>CS(C)=O.C1COCC1>[OH:13][CH:14]([C:20]1[CH:21]=[C:22]([CH:23]=[CH:24][CH:25]=1)[O:26][CH2:2][CH:3]1[CH2:12][CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4]1)[CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]

参加物

7

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 27630372-(Iodomethyl)-1,2,3,4-tetrahydronaphthaleneHCID 117900843-(1-Hydroxyhexyl)phenol

生成物 1

HCID 14257790HCID 14257790、化合物収率 21.3%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 4.0 g (0.018 mol) 2-(iodomethyl)-1,2,3,4-tetrahydronaphthalene, 3.4 g (0.018 mol) 3-(1-hydroxyhexyl)phenol and 3.4 ml NaOH (5N) in 50 ml DMSO and 20 ml THF was stirred at room temperature for a period of 48 hours. The reaction mixture was concentrated under reduced pressure. The concentrated reaction mixture was poured into water and extracted with ether. The ether extract was washed with water, dried over MgSO4 and concentrated to dryness under reduced pressure. The residue was passed through a silica gel comumn using hexane/ethyl acetate (3:1) as eluent. Evaporation of eluent gave an oily product (1.3 g).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customThe concentrated reaction mixture
  3. extractionextracted with ether
  4. extractionThe ether extract
  5. washwas washed with water
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated to dryness under reduced pressure
  8. customEvaporation of eluent

出典と根拠

ORDレコード
ord-5404180083674ffb8296e1910527dae7
出典データセット
uspto-grants-1988_10
特許番号
US04778931

反応ノート

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