HCID 67313552、化合物 → HCID 131729000、化合物

HRID 1010882ノート

反応式

HRID 1010882 の反応式
C(O[C:9](=O)[N:10]([CH2:12][C:13]([C:15]1[CH:20]=[CH:19][C:18]([C@@H:21]([NH:23][C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH3:22])=[CH:17][CH:16]=1)=[O:14])C)C1C=CC=CC=1>O1CCCC1.CO.[C].[Pd]>[C:27]([O:26][C:24](=[O:25])[NH:23][C@H:21]([C:18]1[CH:17]=[CH:16][C:15]([C:13](=[O:14])[CH2:12][NH:10][CH3:9])=[CH:20][CH:19]=1)[CH3:22])([CH3:29])([CH3:28])[CH3:30]

参加物

5

反応物 1

HCID 67313552HCID 67313552、化合物

生成物 1

HCID 131729000HCID 131729000、化合物

試薬・触媒・溶媒 3

HCID 178418390HCID 178418390、化合物触媒2 回HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

159 mg of the compound [2-2] was dissolved in a mixed solvent of 4 mL of tetrahydrofuran and 2 mL of methanol, then 48 mg of 10% palladium carbon catalyst was added thereto, and the mixture was further stirred for 2 hours under hydrogen atmosphere. Thereto, 95 mg of 10% palladium carbon catalyst was further added and stirred for 3.5 hours under hydrogen atmosphere. The insolubles were filtered through celite and the filtrate was concentrated under reduced pressure, to obtain tert-butyl{(1S)-1-[4-(N-methylglycyl)phenyl]ethyl}carbamate [2-3] (hereinafter, referred to as the compound [2-3]) as crude and purified products. The compound [2-3] was used in the subsequent reaction without further purification.

後処理

  1. stirringstirred for 3.5 hours under hydrogen atmosphere
  2. filtrationThe insolubles were filtered through celite
  3. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-ace09b96cbd6480cb26001bb573d6e38
出典データセット
uspto-grants-2011_07
特許番号
US07977336B2

反応ノート

読み込み中…