Epichlorohydrin → HCID 86640177、化合物

HRID 552299ノート

反応式

HRID 552299 の反応式
[OH:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([CH2:9][CH2:10][C:11]([C:13]2[S:14][C:15]([CH2:24][CH2:25][CH3:26])=[C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:17]=2)=[O:12])=[CH:4][C:3]=1[CH3:27].[CH2:28]([CH:30]1[O:32][CH2:31]1)Cl>CC(O)C.[OH-].[Na+].O>[CH3:27][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][C:11]([C:13]2[S:14][C:15]([CH2:24][CH2:25][CH3:26])=[C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:17]=2)=[O:12])[CH:6]=[C:7]([CH3:8])[C:2]=1[O:1][CH2:28][CH:30]1[CH2:31][O:32]1

参加物

6

反応物 2

HCID 7835EpichlorohydrinHCID 592489793-(4-Hydroxy-3,5-dimethyl-phenyl)-1-(4-phenyl-5-propyl-thiophen-2-yl)-propan-1-one

生成物 1

HCID 86640177HCID 86640177、化合物収率 89.5%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3776Isopropanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of 3-(4-hydroxy-3,5-dimethyl-phenyl)-1-(4-phenyl-5-propyl-thiophen-2-yl)-propan-1-one (250 mg, 0.661 mmol) in 2-propanol (2 mL) and 3 N aq. NaOH (1 mL) is treated with epichlorohydrine (122 mg, 1.32 mmol) and the mixture is stirred at rt for 18 h, then diluted with water and extracted with EA. The solvent of the organic extract is evaporated to give crude 3-(3,5-dimethyl-4-oxiranylmethoxy-phenyl)-1-(4-phenyl-5-propyl-thiophen-2-yl)-propan-1-one (257 mg) as a yellow oil; LC-MS: tR=1.18 min, [M+1]+=435.20.

後処理

  1. extractionextracted with EA
  2. extractionThe solvent of the organic extract
  3. customis evaporated

出典と根拠

ORDレコード
ord-6049b2ae6d604a9e9efd5b98f3187169
出典データセット
uspto-grants-2011_05
特許番号
US07951794B2

反応ノート

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