Triethylamine → 1,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-diyl dimethanesulfonate

HRID 1470924노트

반응식

HRID 1470924 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:23])[CH2:9][CH2:10][CH:11]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([N+:20]([O-:22])=[O:21])[CH:14]=2)[OH:12])=[CH:4][C:3]=1[N+:24]([O-:26])=[O:25].C(N(CC)CC)C.[CH3:34][S:35](Cl)(=[O:37])=[O:36]>ClCCl>[CH3:34][S:35]([O:12][CH:11]([C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([N+:20]([O-:22])=[O:21])[CH:14]=1)[CH2:10][CH2:9][CH:8]([O:23][S:35]([CH3:34])(=[O:37])=[O:36])[C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([N+:24]([O-:26])=[O:25])[CH:4]=1)(=[O:37])=[O:36]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 767088951,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-diol

생성물 1

HCID 767087941,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-diyl dimethanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The product of Example 28B (4.81 g, 11.99 mmol) and triethylamine (5.85 mL, 42.0 mmol) were dissolved in dichloromethane (80 mL) at room temperature and treated with methanesulfonyl chloride (2.34 mL, 30.0 mmol) dropwise over 10 minutes. The resulting solution was stirred for 2 h then concentrated to dryness and used directly in the next step.

후처리

  1. concentrationthen concentrated to dryness

출처 및 근거

ORD 기록
ord-52f291a38f054179a5a611d7af64ff58
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006387B2

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