1-Chloro-N,N-2-trimethylpropenylamine → HCID 68501265、化合物

HRID 1176590ノート

反応式

HRID 1176590 の反応式
O[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:16])[CH2:11][CH:10]2[O:25][CH2:26][C:27]2[CH:28]=[CH:29][C:30]3[O:35][CH2:34][CH2:33][N:32]([CH2:36][CH2:37][CH2:38][O:39][CH3:40])[C:31]=3[CH:41]=2)=[CH:5][CH:4]=1.[Cl:42]C(N(C)C)=C(C)C>ClCCl>[Cl:42][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:16])[CH2:11][CH:10]2[O:25][CH2:26][C:27]2[CH:28]=[CH:29][C:30]3[O:35][CH2:34][CH2:33][N:32]([CH2:36][CH2:37][CH2:38][O:39][CH3:40])[C:31]=3[CH:41]=2)=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 6407921-Chloro-N,N-2-trimethylpropenylamineHCID 68501539HCID 68501539、化合物

生成物 1

HCID 68501265HCID 68501265、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The stirred solution of 0.980 g of benzyl 4-(4-hydroxymethylphenyl)-3-[4-(3-methoxypropyl)-3,4-dihydro-2H-benzo[1,4]oxazin-6-ylmethoxy]piperidine-1-carboxylate and 20 ml of dichloromethane is admixed with 2.12 ml of 1-chloro-N,N,2-trimethylpropenylamine (chlorenamine) in portions over 24 hours. The reaction mixture is poured onto water (100 ml) and extracted with tert-butyl methyl ether (100 ml). The organic phase is washed with brine (50 ml), dried over sodium sulphate, filtered and concentrated by evaporation. The title compound is obtained as a slightly yellowish oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.39 (2:1 EtOAc-heptane); Rt=5.57

後処理

  1. additionThe reaction mixture is poured onto water (100 ml)
  2. extractionextracted with tert-butyl methyl ether (100 ml)
  3. washThe organic phase is washed with brine (50 ml)
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-dae497ac7b624e669d14dcb510ac1071
出典データセット
uspto-grants-2010_11
特許番号
US07842688B2

反応ノート

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