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HRID 1470562

반응식

HRID 1470562 반응식
[CH2:1]1[S:3][CH:2]1[CH2:4][Cl:5].O.[N:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C1(C)C=CC=CC=1>[N:7]1[CH:12]=[CH:11][CH:10]=[CH2+:9][CH:8]=1.[Cl-:5].[S:3]1[CH2:2][CH2:4][CH2:1]1

참가 물질

4

반응물 3

HCID 962WaterHCID 1049PyridineHCID 18588Epithiochlorohydrin

생성물 0

아직 생성물 데이터가 없습니다.

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
50 °C

실험 절차

To a solution of epithiochlorohydrin (6.48 g) in toluene (60 mL) were added water (60 mL) and pyridine (23.7 g). The resulting mixture was stirred at 50° C. for 16 h. The two phases were separated and the aqueous phase was then lyophilized to give a yellow oil (13.2 g). The crude oil was filtered over a plug of silica gel, eluting with EtOH:H2O (100:0 to 95:5). The desired salt was obtained as an amber solid was obtained (6.1 g). 1H-NMR (D2O, 500 MHz): 3.59 (t, 2H), 3.91 (t, 2H), 5.99 (dt, 2H), 8.00 (m, 2H), 8.47 (m, 1H), 8.86 (m, 2H). 13C-NMR (D2O, 125 MHz): 32.6 (2C), 63.8, 128.1 (2C), 141.7, 146.5 (2C).

후처리

  1. customThe two phases were separated

출처 및 근거

ORD 기록
ord-21e3ade8e94344b4b3667e77d15de88a
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006456B2

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