Sodium Iodide → 7-Nitro-3,4-dihydro-2H-benzo[b][1,4]thiazine

HRID 424499노트

반응식

HRID 424499 반응식
Cl[CH2:2][CH2:3][S:4][C:5]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:6]=1[NH2:7].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C=O)C.O>[N+:12]([C:10]1[CH:9]=[CH:8][C:6]2[NH:7][CH2:2][CH2:3][S:4][C:5]=2[CH:11]=1)([O-:14])=[O:13]

참가 물질

6

반응물 3

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 591440982-(2-Chloroethylthio)-4-nitroaniline

생성물 1

HCID 204961217-Nitro-3,4-dihydro-2H-benzo[b][1,4]thiazine수율 94%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a stirred solution of 2-(2-chloroethylthio)-4-nitroaniline (5.13 g, 22.05 mmol) in DMF (70 mL) was added potassium carbonate (9.14 g, 66.1 mmol), followed by sodium iodide (0.330 g, 2.205 mmol). The resulting suspension was stirred at room temperature overnight. The mixture was then diluted with water, and the resulting crystals were collected by vacuum filtration, giving the desired product (4.06 g, 94%). 1H NMR (DMSO-d6) δ 7.81-7.73 (m, 3H), 6.58 (t, J=9.0 Hz, 1H), 3.65-3.60 (m, 2H), 3.01-2.97 (m, 2H); ESI-MS (m/z, %): 197 (MH+, 100), 180 (99).

후처리

  1. filtrationthe resulting crystals were collected by vacuum filtration

출처 및 근거

ORD 기록
ord-beec36693adb436fb38bf96dfbc99768
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106043B2

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