Hydrochloric Acid → HCID 12138358, 화합물

HRID 1271668노트

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HRID 1271668 반응식
[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]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 12138357HCID 12138357, 화합물

생성물 1

HCID 12138358HCID 12138358, 화합물수율 10%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5a614f9d2639440d97c3e78c96e425d4
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205428B2

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