참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | Chlorosulfonic acid | HCID 24638 | — |
| 반응물 | 3,5-Dimethylanisole | HCID 70126 | — |
| 반응물 | N-Methylaminoethanol | HCID 5247031 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-(2-Hydroxyethyl)-4-methoxy-N,2,6-trimethylbenzenesulfonamide | HCID 51712110 | — |
반응 단계
10.00 kg (73.42 mol) of 3,5-dimethylanisol (A) were dissolved in 35.0 L of dichloromethane. After cooling to −15±5° C. a solution of 17.46 kg (149.86 mol) of chlorosulphonic acid in 20.0 L dichloromethane was metered in and the mixture was stirred for approx. another 30 minutes at −15±5° C. Then the reaction mixture was metered into a solution of 15.0 kg sodium chloride in 85.0 L of water that had been cooled to −7±5° C., and diluted with 15.0 L of dichloromethane. The organic phase was separated off, diluted with 15.0 L of dichloromethane and washed with 30.0 L of sodium hydrogen carbonate solution (5%). After separation of the organic phase once again and dilution with 10 L of dichloromethane, a solution of 11.58 kg (154.20 mol) N-methylaminoethanol in 10.0 L of dichloromethane was slowly metered in at 10±5° C. After the reaction had ended 45.0 L of HCl (3%) and 5.0 L of water were added. The organic phase was separated off, diluted with 10.0 L dichloromethane and the solvent was totally eliminated from the product (C) in vacuo.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08207335B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
|---|
| ORD ID | ord-9f1f5c869ec84a169535a776eb208804 |
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| 출처 메모 | uspto-grants-2012_06 |
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