Sodium Hydroxide → HCID 54391157, 화합물

HRID 1277572

반응식

HRID 1277572 반응식
[C:1]([C:5]1[C:10]([OH:11])=[C:9]([CH3:12])[C:8]([CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH3:18])=[C:7]([CH3:19])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[C:20]1([S:30](Cl)(=[O:32])=[O:31])[CH:25]=[CH:24][CH:23]=[C:22]([S:26](Cl)(=[O:28])=[O:27])[CH:21]=1.[OH-:34].[Na+]>CC(C)=O.O>[CH2:15]([N:14]([CH2:13][C:8]1[C:9]([CH3:12])=[CH:10][C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])=[C:6]([OH:34])[C:7]=1[CH3:19])[S:30]([C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([S:26]([N:14]([CH2:15][CH2:16][CH2:17][CH3:18])[CH2:13][C:8]2[C:7]([CH3:19])=[CH:6][C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])=[C:10]([OH:11])[C:9]=2[CH3:12])(=[O:28])=[O:27])[CH:21]=1)(=[O:32])=[O:31])[CH2:16][CH2:17][CH3:18]

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 962401,3-Benzenedisulfonyl dichlorideHCID 20574811HCID 20574811, 화합물

생성물 1

HCID 54391157HCID 54391157, 화합물수율 100.1%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

To a stirred solution of 6-t-butyl-3-(butylaminomethyl)-2,4-dimethylphenol (5.26 grams; 0.02 mole) in acetone (40 mls) is slowly added 1,3-benzenedisulfonyl chloride (2.75 grams; 0.01 mole) while maintaining the temperature at 25°-30° C. by cooling. To this mixture is slowly added a solution of 50% caustic soda (1.6 grams; 0.02 mole) in water (22 mls) while maintaining the temperature at 25°-30° C. by cooling. The mixture is allowed to come to room temperature and stirred for 15 hours. The mixture is then allowed to settle, and the upper layer is separated and slowly treated with ice water (100 mls). The resulting oil which separates solidifies upon standing for 2.5 hours. The solid is then recovered by filtration to obtain the crude product (7.3 grams; 100% of theoretical). Recrystallization of the crude product from glacial acetic acid affords the pure product (2.5 grams; m.p. 143°-144.5° C.).

후처리

  1. temperaturewhile maintaining the temperature at 25°-30° C.
  2. temperatureby cooling
  3. temperaturewhile maintaining the temperature at 25°-30° C.
  4. temperatureby cooling
  5. customto come to room temperature
  6. customthe upper layer is separated
  7. additionslowly treated with ice water (100 mls)
  8. waitupon standing for 2.5 hours
  9. filtrationThe solid is then recovered by filtration

출처 및 근거

ORD 기록
ord-939760b5f2914b99835e6e0774665500
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04278577

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