Dichloromethane → HCID 131733089, 화합물

HRID 1518998노트

반응식

HRID 1518998 반응식
Cl[C:2]1[CH:13]=[CH:12][C:5]([C:6]([NH:8][CH:9]([CH3:11])[CH3:10])=[O:7])=[C:4]([NH:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:3]=1.C(N(C(C)C)CC)(C)C.[CH3:31][N:32]1[C:36]([S:37](Cl)(=[O:39])=[O:38])=[CH:35][CH:34]=[N:33]1.[Cl:41]CCl>O>[Cl:41][C:19]1[CH:20]=[CH:21][C:16]([CH2:15][N:14]([C:4]2[CH:3]=[CH:2][CH:13]=[CH:12][C:5]=2[C:6]([NH:8][CH:9]([CH3:11])[CH3:10])=[O:7])[S:37]([C:36]2[N:32]([CH3:31])[N:33]=[CH:34][CH:35]=2)(=[O:39])=[O:38])=[CH:17][CH:18]=1

참가 물질

6

반응물 4

HCID 6344Dichloromethane2회HCID 81531DiisopropylethylamineHCID 224726211-Methyl-1H-pyrazole-5-sulfonyl chlorideHCID 131733090HCID 131733090, 화합물

생성물 1

HCID 131733089HCID 131733089, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

3-(4-Chloro-benzylamino-N-isopropyl-benzamide (30 mg, 0.1 mmol), diisopropylethylamine (35 μL, 0.2 mmol) and 1-methyl-1H-pyrazole-5-sulfonyl chloride (36 mg, 0.2 mmol) were stirred in dry dichloromethane (2 ml) at room temperature for 72 hrs. The reaction was diluted with dichloromethane (5 ml) and water (5 ml) with stirring. The organics were collected, dried (PTFE frit) and concentrated in vacuo. The residue was purified by preparative TLC (10% ethyl acetate/dichloromethane) to yield the product as an off-white solid (11.9 mg). HPLC retention time 8.04 min. Mass spectrum (ES+) m/z 44 (M+H).

후처리

  1. customThe organics were collected
  2. dry with materialdried (PTFE frit)
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by preparative TLC (10% ethyl acetate/dichloromethane)

출처 및 근거

ORD 기록
ord-b3110d3a783e46479a3502e47ca751a4
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073834B2

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