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Hydrochloric Acid → 1-{4-[3-(3,4-Bis-hydroxymethyl-phenyl)-propyl]-2-ethyl-phenoxy}-3,3-dimethyl-butan-2-ol

HRID 970836
ノート
印刷プレビュー

反応式

HRID 970836 の反応式
[CH3:1][C:2]([CH3:33])([CH3:32])[C:3](=[O:31])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][CH2:13][CH2:14][C:15]2[CH:16]=[C:17]([C:25](OC)=[O:26])[C:18](=[CH:23][CH:24]=2)[C:19](OC)=[O:20])=[CH:8][C:7]=1[CH2:29][CH3:30].[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+].Cl>C1COCC1.O>[OH:26][CH2:25][C:17]1[CH:16]=[C:15]([CH2:14][CH2:13][CH2:12][C:9]2[CH:10]=[CH:11][C:6]([O:5][CH2:4][CH:3]([OH:31])[C:2]([CH3:32])([CH3:33])[CH3:1])=[C:7]([CH2:29][CH3:30])[CH:8]=2)[CH:24]=[CH:23][C:18]=1[CH2:19][OH:20]
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 14798Sodium HydroxideHCID 17982979Dimethyl 4-[3-[4-(3,3-dimethyl-2-oxobutoxy)-3-ethylphenyl]propyl}phthalateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 104536321-{4-[3-(3,4-Bis-hydroxymethyl-phenyl)-propyl]-2-ethyl-phenoxy}-3,3-dimethyl-butan-2-ol

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
2 回
HCID 8028Tetrahydrofuran溶媒

実験手順

900 mg (2 mmol) of dimethyl 4-{3-[4-(3,3-dimethyl-2-oxobutoxy)-3-ethylphenyl]propyl}phthalate are dissolved in 20 ml of THF, and slowly added to a suspension of 375 mg (10 mmol) of lithium aluminum hydride. The reaction medium is stirred for 30 minutes at room temperature, and is then sequentially treated by slow addition of 400 μl of water, 400 μl of 15% sodium hydroxide and 1 ml of water. The reaction medium is poured into a 1% hydrochloric acid solution, and then extracted with ethyl ether. The residue obtained after drying and concentrating is purified by chromatography on a silica column. A thick colorless oil is obtained (m=760 mg, y=95%).

後処理

  1. extractionextracted with ethyl ether
  2. customThe residue obtained
  3. customafter drying
  4. concentrationconcentrating
  5. customis purified by chromatography on a silica column
  6. customA thick colorless oil is obtained (m=760 mg, y=95%)

出典と根拠

ORDレコード
ord-f79a07a054bb474f97ee352cfbb37a5f
出典データセット
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07312249B2

反応ノート

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