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Chlorotrimethylsilane → HCID 58513582, 화합물

HRID 241642
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HRID 241642 반응식
[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([S:14]([CH2:17][CH:18]4[CH2:23][CH2:22][N:21](C(OC(C)(C)C)=O)[CH2:20][CH2:19]4)(=[O:16])=[O:15])=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:31][C:32]([CH3:35])([CH3:34])[CH3:33])[CH2:3][CH2:2]1.Cl[Si](C)(C)C>CO>[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([S:14]([CH2:17][CH:18]4[CH2:19][CH2:20][NH:21][CH2:22][CH2:23]4)(=[O:15])=[O:16])=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:31][C:32]([CH3:35])([CH3:34])[CH3:33])[CH2:2][CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6397ChlorotrimethylsilaneHCID 58513612HCID 58513612, 화합물

생성물 1

HCID 58513582HCID 58513582, 화합물수율 73%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of tert-butyl 4-((1-(cyclopropylmethyl)-2-neopentyl-1H-benzo[d]imidazol-5-ylsulfonyl)methyl)piperidine-1-carboxylate (STEP C, 1.39 g, 2.76 mmol) in methanol (15 mL) was added chlorotrimethylsilane (1.41 mL, 11.0 mmol). After stirring for 18 h, the mixture was concentrated in vacuo. The residue was diluted ethyl acetate and basified with saturated sodium bicarbonate aqueous solution. The aqueous layer was extracted with ethyl acetate and the combined organic layers were dried over sodium sulfate and concentrated to give the title compound (809 mg, 73%) as an amorphous.

후처리

  1. concentrationthe mixture was concentrated in vacuo
  2. extractionThe aqueous layer was extracted with ethyl acetate
  3. dry with materialthe combined organic layers were dried over sodium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0c7f29696d6746699616570ad2d84300
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08653063B2

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