Glycine, N-methyl-, methyl ester, hydrochloride (1:1) → HCID 66676715、化合物

HRID 423278

反応式

HRID 423278 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 66676715HCID 66676715、化合物収率 73.1%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-307f78e7a06f4762a4fb51a752d817c5
出典データセット
uspto-grants-2012_01
特許番号
US08101774B2

関連ノート

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