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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
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HRID 970836 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 17982979Dimethyl 4-[3-[4-(3,3-dimethyl-2-oxobutoxy)-3-ethylphenyl]propyl}phthalateHCID 21226445Aluminium lithium hydride

생성물 1

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

시약·촉매·용매 2

HCID 962
Water
용매
2회
HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-f79a07a054bb474f97ee352cfbb37a5f
출처 데이터셋
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07312249B2

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