Hydrochloric Acid → 3-Methyl-5-(3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydro-naphthalen-2-ylsulphonyl)pent-2-en-4-ynoic Acid

HRID 897066ノート

反応式

HRID 897066 の反応式
[OH-].[Na+].[CH3:3][C:4]([C:11]#[C:12][S:13]([C:16]1[C:25]([CH3:26])=[CH:24][C:23]2[C:22]([CH3:28])([CH3:27])[CH2:21][CH2:20][C:19]([CH3:30])([CH3:29])[C:18]=2[CH:17]=1)(=[O:15])=[O:14])=[CH:5][C:6]([O:8]CC)=[O:7].C(OCC)C.O.Cl>C1COCC1>[CH3:3][C:4]([C:11]#[C:12][S:13]([C:16]1[C:25]([CH3:26])=[CH:24][C:23]2[C:22]([CH3:28])([CH3:27])[CH2:21][CH2:20][C:19]([CH3:30])([CH3:29])[C:18]=2[CH:17]=1)(=[O:15])=[O:14])=[CH:5][C:6]([OH:8])=[O:7]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21584184Diethylether waterHCID 73884431Ethyl 3-methyl-5-(3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydronaphthalen-2-ylsulphonyl)pent-2-en-4-ynoate

生成物 1

HCID 738844293-Methyl-5-(3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydro-naphthalen-2-ylsulphonyl)pent-2-en-4-ynoic Acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Sodium hydroxide (400 mg, 10 mmol) is added to a solution of ethyl 3-methyl-5-(3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydronaphthalen-2-ylsulphonyl)pent-2-en-4-ynoate (400 mg, 1.6 mmol) in 15 ml of THF. The medium is refluxed for 4 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. The residue is then triturated from heptane, after which it is filtered.

後処理

  1. temperatureThe medium is refluxed for 4 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
  7. customThe residue is then triturated from heptane
  8. filtrationafter which it is filtered

出典と根拠

ORDレコード
ord-fc08218ce36547aabca2599af7d8725d
出典データセット
uspto-grants-2005_07
特許番号
US06921777B2

反応ノート

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