Hydrochloric Acid → Cgp-7930

HRID 372592

반응식

HRID 372592 반응식
[OH-].[Na+].[OH-].C([N+](C)(C)C)C1C=CC=CC=1.[C:15]([C:19]1[CH:20]=[C:21]([CH:24]=[C:25]([C:28]([CH3:31])([CH3:30])[CH3:29])[C:26]=1[OH:27])[CH2:22]Cl)([CH3:18])([CH3:17])[CH3:16].[CH:32](=[O:36])[CH:33]([CH3:35])[CH3:34].C(Cl)C1C=CC=CC=1.C(=O)C(C)C.Cl>C1C=CC=CC=1.O.C1C=CC=CC=1.O>[CH3:34][C:33]([CH3:35])([CH2:22][C:21]1[CH:20]=[C:19]([C:15]([CH3:18])([CH3:17])[CH3:16])[C:26]([OH:27])=[C:25]([C:28]([CH3:31])([CH3:30])[CH3:29])[CH:24]=1)[CH2:32][OH:36]

참가 물질

10

반응물 6

HCID 313Hydrochloric AcidHCID 6561IsobutyraldehydeHCID 14798Sodium HydroxideHCID 66854Benzyltrimethylammonium hydroxideHCID 123786012,6-Di-tert-butyl-4-(chloromethyl)phenolHCID 86735727Benzyl chloride isobutyraldehyde

생성물 1

HCID 5024764Cgp-7930수율 103%

시약·촉매·용매 3

HCID 241Benzene용매3회HCID 962Water용매2회HCID 22272175Benzene--water (1/1)용매

실험 절차

A three-neck, three-liter flask equipped with a mechanical stirrer, thermometer and an addition funnel was charged with 80 grams of sodium hydroxide and 80 milliliters of water under a nitrogen atmosphere. The mixture was stirred until dissolved and a mixture of 450 milliliters of benzene and 12.5 milliliters of 40 percent methanolic benzyl trimethyl ammonium hydroxide was added forming a benzene-water mixture. A mixture of 383 grams of 3,5-di-t-butyl-4-hydroxy benzyl chloride and 144 grams of isobutyraldehyde was prepared and placed in the addition funnel. The benzyl chloride/isobutyraldehyde mixture was added to the mixture of benzene and water while the flask contents were vigorously stirred at a temperature of 50° C to 60° C over a two-hour period. After addition was complete, the mixture was stirred for an additional one-half hour at room temperature. The mixture was hydrolyzed with dilute hydrochloric acid until the benzene layer turned clear yellow-orange color. The benzene layer was separated and the benzene evaporated to obtain 453 grams of 2,2-di-methyl-3-(3,5-di-t-butyl-4-hydroxyphenyl)propanol. The melting point of the product was between 72° C and 74° C after recrystalization from hexane.

후처리

  1. customA three-neck, three-liter flask equipped with a mechanical stirrer
  2. dissolutionuntil dissolved
  3. additionwas added
  4. customwas prepared
  5. stirringwere vigorously stirred at a temperature of 50° C to 60° C over a two-hour period
  6. additionAfter addition
  7. stirringthe mixture was stirred for an additional one-half hour at room temperature
  8. customThe benzene layer was separated
  9. customthe benzene evaporated

출처 및 근거

ORD 기록
ord-0bdf1cce1ad341f28a2daab9514671b1
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04091225

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