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Hydrochloric Acid → HCID 14726488, 화합물

HRID 1728465
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HRID 1728465 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

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

생성물 1

HCID 14726488HCID 14726488, 화합물수율 56.3%

시약·촉매·용매 3

HCID 962Water
용매
2회
HCID 1140Toluene용매2회
HCID 80711,2-Dimethoxyethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fc6b59dc31a144f9b423e8e400c8a1f9
출처 데이터셋
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05326900

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