Water → 4-chloro-N-hexadecyl-N-methyl-3-nitrobenzenesulfonamide

HRID 728524ノート

反応式

HRID 728524 の反応式
[CH2:1]([NH:17][S:18]([C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([N+:28]([O-:30])=[O:29])[CH:22]=1)(=[O:20])=[O:19])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].[C:31](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O.O>CC(C)=O>[CH3:31][N:17]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[S:18]([C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([N+:28]([O-:30])=[O:29])[CH:22]=1)(=[O:19])=[O:20]

参加物

6

反応物 4

HCID 962WaterHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 14324551HCID 14324551、化合物

生成物 1

HCID 41628334-chloro-N-hexadecyl-N-methyl-3-nitrobenzenesulfonamide収率 97%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

170 g of N-hexadecyl-3-nitro-4-chlorobenzenesulfonamide was dissolved in 640 ml of acetone, and thereto were added 79 g of potassium carbonate, 6 ml of Polyethylene Glycol 400 and 71 g of dimethyl sulfate. The resulting mixture was heated under reflux for 5 hours. To the resulting reaction mixture, 240 ml of acetone was added, and then 870 ml of water was added dropwise. Upon cooling to room temperature, crystals were deposited. The crystals were filtered off, washed successively with water and methanol, and then dried. Yield: 169 g, Percent yield: 97%, Melting point: 74°-75° C.

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 5 hours
  3. additionwas added
  4. filtrationThe crystals were filtered off
  5. washwashed successively with water and methanol
  6. customdried

出典と根拠

ORDレコード
ord-f8f07d5c8c6f4eaa8fb3b8b1acdc3a0b
出典データセット
uspto-grants-1991_09
特許番号
US05049477

反応ノート

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