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Hydrochloric Acid → HCID 14726488、化合物

HRID 1614093
ノート
印刷プレビュー

反応式

HRID 1614093 の反応式
[C:1]([O:13]C)(=O)[C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.[C:15]([C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][CH:27]=1)[C:24]([CH3:29])([CH3:28])[CH2:23][CH2:22][C:21]2([CH3:31])[CH3:30])(=[O:17])[CH3:16].[H-].[Na+].Cl>C1(C)C=CC=CC=1.C(COC)OC.O>[C:6]([C:5]1[CH:4]=[CH:3][C:2]([C:1](=[O:13])[CH2:16][C:15]([C:18]2[CH:27]=[CH:26][C:25]3[C:24]([CH3:29])([CH3:28])[CH2:23][CH2:22][C:21]([CH3:31])([CH3:30])[C:20]=3[CH:19]=2)=[O:17])=[CH:11][CH:10]=1)([O:8][CH3:9])=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 8441Dimethyl terephthalateHCID 24758Sodium hydrideHCID 27475621-(5,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)ethan-1-one

生成物 1

HCID 14726488HCID 14726488、化合物収率 56.3%

試薬・触媒・溶媒 3

HCID 962Water
溶媒
2 回
HCID 1140Toluene溶媒2 回
HCID 80711,2-Dimethoxyethane溶媒

実験手順

A solution of 19.4 g (0.1 mol) of dimethyl terephthalate and 23 g (0.1 mol) of 6-acetyl-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene in 80 ml of toluene and 20 ml of dimethoxyethane was added dropwise under nitrogen to a suspension of 3.6 g (0.15 mol) of sodium hydride in 21 ml of toluene at 100° C. The mixture was refluxed for 5 h and, after cooling, 50 ml of water were added, and the mixture was acidified with 50% concentrated hydrochloric acid, poured into 500 ml of water and extracted with chloroform. The precipitated product was filtered off with suction, and the chloroform phase was dried over sodium sulfate and concentrated. The residue and crude product were mixed and washed several times with hot methanol. Drying of the crystals resulted in 22.1 g of the title compound of melting point 128° C.

後処理

  1. temperatureThe mixture was refluxed for 5 h
  2. temperatureafter cooling
  3. extractionextracted with chloroform
  4. filtrationThe precipitated product was filtered off with suction
  5. dry with materialthe chloroform phase was dried over sodium sulfate
  6. concentrationconcentrated
  7. additionThe residue and crude product were mixed
  8. washwashed several times with hot methanol
  9. customDrying of the crystals

出典と根拠

ORDレコード
ord-063302eae94349b4b04cf28af8ee752a
出典データセット
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05194664

反応ノート

読み込み中…

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