Benzhydrylamine → HCID 21998158、化合物

HRID 1977492ノート

反応式

HRID 1977492 の反応式
O.[C:2]([OH:6])(=[O:5])[CH:3]=O.[NH2:7][CH:8]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[C:21]1(B(O)O)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>ClCCl>[C:15]1([CH:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[NH:7][CH:3]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:2]([OH:6])=[O:5])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 7036BenzhydrylamineHCID 66827Phenylboronic AcidHCID 15620607Glyoxylic acid, monohydrate

生成物 1

HCID 21998158HCID 21998158、化合物収率 84%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of glyoxylic acid monohydrate (92 mg, 1 mmol) in dichloromethane (7 mL) was added aminodiphenylmethane (183 mg, 1 mmol), followed by phenylboronic acid (122 mg, 1 mmol). After the flask was purged with argon and sealed, the reaction mixture was stirred vigorously at room temperature for 48 h. The resulting precipitate was isolated by filtration, washed with dichloromethane (10 mL) and purified by ion-exchange chromatography (Dowex 50W-X8) to give pure (±)-N-(diphenylmethyl)-α-phenylglycine (266 mg, 84% yield).

後処理

  1. customAfter the flask was purged with argon
  2. customsealed
  3. customThe resulting precipitate was isolated by filtration
  4. washwashed with dichloromethane (10 mL)
  5. custompurified by ion-exchange chromatography (Dowex 50W-X8)

出典と根拠

ORDレコード
ord-61843cf72a83446ea3c43395d1058ee2
出典データセット
uspto-grants-2001_05
特許番号
US06232467B1

反応ノート

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