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

HRID 728524노트

반응식

HRID 728524 반응식
[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]

참가 물질

6

반응물 4

HCID 962WaterHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 14324551HCID 14324551, 화합물

생성물 1

HCID 41628334-chloro-N-hexadecyl-N-methyl-3-nitrobenzenesulfonamide수율 97%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f8f07d5c8c6f4eaa8fb3b8b1acdc3a0b
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05049477

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