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Hydrochloric Acid → HCID 9865770、化合物

HRID 1612010
ノート
印刷プレビュー

反応式

HRID 1612010 の反応式
[OH-].[Na+].[CH3:3][C:4]1[C:5]([Se:18][C:19]2[CH:29]=[CH:28][C:22]([C:23]([O:25]CC)=[O:24])=[CH:21][CH:20]=2)=[CH:6][C:7]2[C:8]([CH3:17])([CH3:16])[CH2:9][CH2:10][C:11]([CH3:15])([CH3:14])[C:12]=2[CH:13]=1.CO.Cl>C1COCC1.C(OCC)C.O.O>[CH3:3][C:4]1[C:5]([Se:18][C:19]2[CH:20]=[CH:21][C:22]([C:23]([OH:25])=[O:24])=[CH:28][CH:29]=2)=[CH:6][C:7]2[C:8]([CH3:17])([CH3:16])[CH2:9][CH2:10][C:11]([CH3:14])([CH3:15])[C:12]=2[CH:13]=1
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 887MethanolHCID 14798Sodium HydroxideHCID 9867289HCID 9867289、化合物

生成物 1

HCID 9865770HCID 9865770、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8028
Tetrahydrofuran
溶媒
HCID 21584184Diethylether water溶媒

実験手順

Sodium hydroxide (450 mg, 11.25 mmol) is added to a solution of ethyl 4-(3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydro-2-naphthylselanyl)benzoate (450 mg, 1.04 mmol) in a mixture of 10 ml of THF, 1 ml of methanol and 1 ml of water. The reaction medium is refluxed for 12 h. It is then poured into an ethyl ether/water mixture, acidified to pH 1 with concentrated hydrochloric acid solution and extracted with ethyl ether. After separation of the phases by settling, the organic phase is washed twice with water, dried over anhydrous magnesium sulphate and concentrated on a rotary evaporator under vacuum at 40° C.

後処理

  1. temperatureThe reaction medium is refluxed for 12 h
  2. extractionextracted with ethyl ether
  3. customAfter separation of the phases
  4. washthe organic phase is washed twice with water
  5. dry with materialdried over anhydrous magnesium sulphate
  6. concentrationconcentrated on a rotary evaporator under vacuum at 40° C.

出典と根拠

ORDレコード
ord-ea09d407f2a34a67a5b35a210aa852c1
出典データセット
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06992094B1

反応ノート

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