Triethylamine → HCID 66953038、化合物

HRID 1593478ノート

反応式

HRID 1593478 の反応式
N[C@H:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][C@@H:3]1[C:15]([O:17][CH3:18])=[O:16].C(N([CH2:24][CH3:25])CC)C>ClCCl>[CH2:11]([O:10][C:8]([C@H:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][C@H:3]1[C:15]([O:17][CH3:18])=[O:16])=[O:9])[C:25]1[CH:24]=[CH:4][CH:3]=[CH:2][CH:7]=1

参加物

4

反応物 2

HCID 8471TriethylamineHCID 10934154HCID 10934154、化合物

生成物 1

HCID 66953038HCID 66953038、化合物収率 184.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 260B (0.75 g, 2.90 mmol) in dichloromethane (30 mL) at 0° C. was treated with triethylamine (0.35 g, 3.48 mmol) and N-(benzyloxycarbonyoxy)succinimide (0.72 g, 2.90 mmol). The reaction mixture was allowed to warm to room temperature and was stirred for 16 hours. The reaction mixture was diluted with dichloromethane, washed with 10% citric acid (2×50 mL), then saturated NaHCO3 (2×50 mL). The organic layer was dried over Na2SO4 and concentrated in vacuo to give 1.01 g (yield: 89%) of Compound 260C as an oil. It was used in the next step without further purification.

後処理

  1. washwashed with 10% citric acid (2×50 mL)
  2. dry with materialThe organic layer was dried over Na2SO4
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-a5f3f3e728544f389ac552fb4e59a3bb
出典データセット
uspto-grants-2007_11
特許番号
US07297695B2

反応ノート

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