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2-Bromophenyl isocyanate → SB705498

HRID 559485
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인쇄 미리보기

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HRID 559485 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]=[C:9]=[O:10].[F:11][C:12]([F:26])([F:25])[C:13]1[CH:14]=[CH:15][C:16]([N:19]2[CH2:23][CH2:22][C@@H:21]([NH2:24])[CH2:20]2)=[N:17][CH:18]=1>C(OCC)C>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]([NH:24][C@@H:21]1[CH2:22][CH2:23][N:19]([C:16]2[CH:15]=[CH:14][C:13]([C:12]([F:26])([F:25])[F:11])=[CH:18][N:17]=2)[CH2:20]1)=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1370972-Bromophenyl isocyanateHCID 11401990HCID 11401990, 화합물

생성물 1

HCID 9910486SB705498

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of 2-bromophenyl isocyanate (Aldrich Chemical Company) (27.4 ml, 0.222 mol) in dry diethyl ether (65 ml) was added dropwise over 0.5 h to an efficiently stirred solution of D2 (51.4 g, 0.222 mol) in dry diethyl ether (0.8 L) under argon at ambient temperature. After stirring for 18 h, a white precipitate was filtered off and washed with dry diethyl ether (2×150 ml). The solid was crushed to a fine powder and then re-stirred with diethyl ether (470 ml) for 4 h at ambient temperature. The insoluble product was filtered off, washed with diethyl ether (100 ml) and dried at 50° C./vacuum/24 h to afford title compound as a white solid.

후처리

  1. filtrationa white precipitate was filtered off
  2. washwashed with dry diethyl ether (2×150 ml)
  3. customThe solid was crushed to a fine powder
  4. stirringre-stirred with diethyl ether (470 ml) for 4 h at ambient temperature
  5. filtrationThe insoluble product was filtered off
  6. washwashed with diethyl ether (100 ml)
  7. customdried at 50° C./vacuum/24 h

출처 및 근거

ORD 기록
ord-d3511f7a09124aa1bdc5326d9f48a13d
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08063078B2

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