Dichloromethane → HCID 67345002、化合物

HRID 2036879ノート

反応式

HRID 2036879 の反応式
Cl.[CH2:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12]([O:14][CH3:15])=[O:13])=[CH:9][CH:10]=2)[CH2:5][CH2:4][NH:3]1.C(N(CC)CC)C.ClCCl.Cl[C:27]([O:29][CH2:30][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)=[O:28]>CN(C1C=CN=CC=1)C.O>[CH2:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12]([O:14][CH3:15])=[O:13])=[CH:9][CH:10]=2)[CH2:5][CH2:4][N:3]1[C:27]([O:29][CH2:30][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)=[O:28]

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 42614607Methyl 1,2,3,4-tetrahydroisoquinoline-6-carboxylate hydrochloride

生成物 1

HCID 67345002HCID 67345002、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

A mixture of 10 g methyl 1,2,3,4-tetrahydroisoquinoline-6-carboxylate hydrochloride, 10 ml triethylamine, and 15 ml dichloromethane with 525 mg DMAP is stirred at 0° C. and 9.3 ml of benzyl chloroformate are added dropwise. After stirring overnight at ambient temperature, the reaction mixture is added to cold water. The organic phase is washed, dried, and evaporated. The crude product is purified by a silica gel chromatography.

後処理

  1. stirringAfter stirring overnight at ambient temperature
  2. washThe organic phase is washed
  3. customdried
  4. customevaporated
  5. customThe crude product is purified by a silica gel chromatography

出典と根拠

ORDレコード
ord-a6f8ec461b1c474186b1886233d3c357
出典データセット
uspto-grants-2013_11
特許番号
US08575193B2

反応ノート

読み込み中…