Glycine, N-methyl-, methyl ester, hydrochloride (1:1) → HCID 66676715, 화합물

HRID 423278

반응식

HRID 423278 반응식
[CH3:1][N:2]([CH3:32])[C:3]([C:5]1[CH:10]=[C:9]([CH:11]=O)[CH:8]=[CH:7][C:6]=1[NH:13][C:14]([C:16]1[C:17]([C:22]2[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][CH:23]=2)=[CH:18][CH:19]=[CH:20][CH:21]=1)=[O:15])=[O:4].Cl.[CH3:34][O:35][C:36](=[O:40])[CH2:37][NH:38][CH3:39].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCl.C(OCC)(=O)C>[CH3:34][O:35][C:36](=[O:40])[CH2:37][NH:38][CH2:39][CH2:11][C:9]1[CH:8]=[CH:7][C:6]([NH:13][C:14]([C:16]2[C:17]([C:22]3[CH:27]=[CH:26][C:25]([C:28]([F:30])([F:31])[F:29])=[CH:24][CH:23]=3)=[CH:18][CH:19]=[CH:20][CH:21]=2)=[O:15])=[C:5]([C:3](=[O:4])[N:2]([CH3:1])[CH3:32])[CH:10]=1

참가 물질

6

반응물 3

HCID 83544Glycine, N-methyl-, methyl ester, hydrochloride (1:1)HCID 5049666Sodium triacetoxyborohydrideHCID 86604648HCID 86604648, 화합물

생성물 1

HCID 66676715HCID 66676715, 화합물수율 73.1%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4′-trifluoromethylbiphenyl-2-carboxylic acid (2-dimethylcarbamoyl-4-formylphenyl)amide (137 mg) and N-methylglycine methyl ester hydrochloride (45 mg) in dichloromethane (2 mL) was added sodium triacetoxyborohydride (97 mg). The mixture was stirred at room temperature for 4 hours, diluted with ethyl acetate, washed successively with saturated aqueous sodium bicarbonate and saturated brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The residue was purified by column chromatography on silica gel (chloroform:methanol=100:1, v/v) to give the title compound (120 mg).

후처리

  1. washwashed successively with saturated aqueous sodium bicarbonate and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by column chromatography on silica gel (chloroform

출처 및 근거

ORD 기록
ord-307f78e7a06f4762a4fb51a752d817c5
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101774B2

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