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Triethylamine → (1-[4-(2-Acetylamino-4-methyl-thiazol-5-yl)-5-bromo-thiophene-2-sulfonyl]-piperidin-4-yl}-methyl-carbamic acid tert-butyl ester

HRID 1948425
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인쇄 미리보기

반응식

HRID 1948425 반응식
[C:1]([NH:4][C:5]1[S:6][C:7]([C:11]2[CH:12]=[C:13]([S:17](Cl)(=[O:19])=[O:18])[S:14][C:15]=2[Br:16])=[C:8]([CH3:10])[N:9]=1)(=[O:3])[CH3:2].C(N(CC)CC)C.[C:28]([O:32][C:33](=[O:42])[N:34]([CH3:41])[CH:35]1[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]1)([CH3:31])([CH3:30])[CH3:29]>C(Cl)Cl>[C:28]([O:32][C:33](=[O:42])[N:34]([CH:35]1[CH2:36][CH2:37][N:38]([S:17]([C:13]2[S:14][C:15]([Br:16])=[C:11]([C:7]3[S:6][C:5]([NH:4][C:1](=[O:3])[CH3:2])=[N:9][C:8]=3[CH3:10])[CH:12]=2)(=[O:19])=[O:18])[CH2:39][CH2:40]1)[CH3:41])([CH3:31])([CH3:29])[CH3:30]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27568064-N-Boc-4-N-Methyl-aminopiperidineHCID 866231464-[2-(Acetylamino)-4-methyl-1,3-thiazol-5-yl]-5-bromothiophene-2-sulfonylchloride

생성물 1

HCID 86652444(1-[4-(2-Acetylamino-4-methyl-thiazol-5-yl)-5-bromo-thiophene-2-sulfonyl]-piperidin-4-yl}-methyl-carbamic acid tert-butyl ester

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

4-[2-(acetylamino)-4-methyl-1,3-thiazol-5-yl]-5-bromothiophene-2-sulfonyl chloride, prepared as in Step III of Example 23 (300 mg; 0.72 mmol; 1 eq), is dissolved in anhydrous DCM (20 ml). The reaction mixture is put under nitrogen. Triethylamine (0.5 ml; 3.61 mmol; 5 eq) and methyl-piperidine-4-yl-carbamic acid tert-butyl ester (773.2 mg; 3.61 mmol; 5 eq) are added successively and the reaction mixture is stirred for 30 minutes at room temperature. It is then washed with water, NaHCO3 sat., brine and dried over MgSO4, affording the title compound (470 mg; quantitative).

후처리

  1. washIt is then washed with water, NaHCO3 sat., brine
  2. dry with materialdried over MgSO4

출처 및 근거

ORD 기록
ord-33b8decf2ebb47ceae338063d2e8230a
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08399497B2

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