Sodium Hydroxide → HCID 54391157、化合物

HRID 1277572

反応式

HRID 1277572 の反応式
[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]

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 962401,3-Benzenedisulfonyl dichlorideHCID 20574811HCID 20574811、化合物

生成物 1

HCID 54391157HCID 54391157、化合物収率 100.1%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-939760b5f2914b99835e6e0774665500
出典データセット
uspto-grants-1981_07
特許番号
US04278577

関連ノート

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