참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1,3-Benzenediamine, N1,N1-dimethyl-, hydrochloride (1:2) | HCID 77124 | — |
| 반응물 | Triphosgene | HCID 94429 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-Dimethylaminophenyl isocyanate | HCID 11789527 | — |
반응 단계
1.46 g (7 mmol) of N1,N1-dimethylbenzene-1,3-diamine dihydrochloride, followed by 9.9 cm3 (71.64 mmol) of triethylamine, are added, at a temperature in the region of 5° C., under an argon atmosphere, to 2.82 g (9.5 mmol) of triphosgene in solution in 150 cm3 of dichloromethane. After stirring for 20 hours at a temperature in the region of 20° C., the reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa), to give a residue which is triturated in 50 cm3 of tetrahydrofuran. After filtration, a solution of 3-dimethylaminophenyl isocyanate in approximately 0.14 N tetrahydrofuran is obtained, which solution is used directly in the subsequent step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07566736B2 |
|---|
| 출처 데이터셋 | uspto-grants-2009_07 |
|---|
| ORD ID | ord-bf812353ccc34e29a55bbe348f993373 |
|---|
| 출처 메모 | uspto-grants-2009_07 |
|---|