Chlorotrimethylsilane → HCID 66780891, 화합물

HRID 1424310

반응식

HRID 1424310 반응식
[F:1][C:2]1[C:7]([F:8])=[C:6]([C:9]2[S:10][CH:11]=[CH:12][CH:13]=2)[C:5]([NH2:14])=[C:4]([NH2:15])[C:3]=1[C:16]1[S:17][CH:18]=[CH:19][CH:20]=1.[S:21](=NC1C=CC=CC=1)=O.Cl[Si](C)(C)C>N1C=CC=CC=1>[F:8][C:7]1[C:2]([F:1])=[C:3]([C:16]2[S:17][CH:18]=[CH:19][CH:20]=2)[C:4]2=[N:15][S:21][N:14]=[C:5]2[C:6]=1[C:9]1[S:10][CH:11]=[CH:12][CH:13]=1

참가 물질

5

반응물 3

HCID 6397ChlorotrimethylsilaneHCID 70739Benzenamine, N-sulfinyl-HCID 86670674HCID 86670674, 화합물

생성물 1

HCID 66780891HCID 66780891, 화합물수율 99.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
80 °C

실험 절차

2,3-difluoro-1,4-di(2-thienyl)-5,6-diamino-benzene (1.2 g, 3.9 mmol) was added into a small flask and purged with Ar three times. Then, dry pyridine (24 ml), N-thionylaniline (1.08 g, 7.8 mmol) and chlorotrimethylsilane (0.76 g, 7.0 mmol) were added. The mixture was stirred at 80° C. for 16 h before poured into ice water. The yellow precipitate was then filtered and washed with a mixture of ethanol and water (1:1 v/v) to afford 5,6-difluoro-4,7-di(2-thienyl)-2,1,3-benzothiadiazole as a yellow solid (1.3 g, 98%). 1H and 19F NMR spectra were as expected.

후처리

  1. custompurged with Ar three times
  2. filtrationThe yellow precipitate was then filtered
  3. washwashed with a mixture of ethanol and water (1:1 v/v)

출처 및 근거

ORD 기록
ord-25d68aae430148d3b11dbd5e66c1a1ae
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08927684B2

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