Hydrochloric Acid → HCID 12138358、化合物

HRID 1271668ノート

反応式

HRID 1271668 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH:36]=[C:37]([C:39]([CH3:42])([CH3:41])[CH3:40])[CH:38]=1)[CH2:8][S:9][C:10]1[CH:11]=[C:12]([CH:17]=[C:18]([S:20][CH2:21][C:22]2[CH:27]=[C:26]([C:28]([CH3:31])([CH3:30])[CH3:29])[CH:25]=[C:24]([C:32]([CH3:35])([CH3:34])[CH3:33])[CH:23]=2)[CH:19]=1)[C:13](OC)=[O:14])([CH3:4])([CH3:3])[CH3:2].Cl>C1(C)C=CC=CC=1>[C:32]([C:24]1[CH:23]=[C:22]([CH:27]=[C:26]([C:28]([CH3:31])([CH3:30])[CH3:29])[CH:25]=1)[CH2:21][S:20][C:18]1[CH:17]=[C:12]([CH:11]=[C:10]([S:9][CH2:8][C:7]2[CH:6]=[C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[CH:38]=[C:37]([C:39]([CH3:42])([CH3:41])[CH3:40])[CH:36]=2)[CH:19]=1)[CH2:13][OH:14])([CH3:35])([CH3:33])[CH3:34]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 12138357HCID 12138357、化合物

生成物 1

HCID 12138358HCID 12138358、化合物収率 10%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

Methyl 3,5-bis(3,5-di-tertiary-butylbenzylthio)benzoate (52.0 g, 86.0 mmol) was dissolved in 300 ml of toluene. To this, was added dropwise a 70% solution of sodium dihydrobis(2-methoxyethoxy)aluminate in toluene (52 g, 180.0 mmol), maintaining the temperature at 35° C. or below and the resulting mixture was stirred for 2 hours under the same conditions. After completion of the reaction, the reaction mixture was poured into 500 ml of a cold 10% hydrochloric acid solution, followed by stirring for 10 minutes. The toluene layer was separated, dried over anhydrous magnesium sulfate and then concentrated. The resulting residue was then purified by means of chromatography with dichloromethane, giving 4.96 g of 3,5-bis(3,5-di-tertiary-butylbenzylthio)benzyl alcohol as a viscous substance.

後処理

  1. temperaturemaintaining the temperature at 35° C. or below
  2. customAfter completion of the reaction
  3. stirringby stirring for 10 minutes
  4. customThe toluene layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe resulting residue was then purified by means of chromatography with dichloromethane

出典と根拠

ORDレコード
ord-5a614f9d2639440d97c3e78c96e425d4
出典データセット
uspto-grants-2007_04
特許番号
US07205428B2

反応ノート

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