Dichloromethane → Ajg-049

HRID 365314ノート

反応式

HRID 365314 の反応式
[CH3:1][O:2][C:3]1[CH:31]=[CH:30][C:6]([CH2:7][CH2:8][N:9]2[CH2:13][CH2:12][CH2:11][C@@H:10]2[CH2:14][N:15]2[C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=3[CH2:19][O:18][C:17]3[CH:26]=[CH:27][CH:28]=[CH:29][C:16]2=3)=[CH:5][CH:4]=1.[Cl:32]CCl>>[ClH:32].[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][CH2:8][N:9]2[CH2:13][CH2:12][CH2:11][C@@H:10]2[CH2:14][N:15]2[C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=3[CH2:19][O:18][C:17]3[CH:26]=[CH:27][CH:28]=[CH:29][C:16]2=3)=[CH:30][CH:31]=1

参加物

3

反応物 2

HCID 6344DichloromethaneHCID 9823094Dibenz(b,E)(1,4)oxazepine, 5,11-dihydro-5-(((2R)-1-(2-(4-methoxyphenyl)ethyl)-2-pyrrolidinyl)methyl)-

生成物 1

HCID 11974305Ajg-049収率 93%

実験手順

A hydrogen chloride ether saturated solution was added to a solution of 2.9 g (7.0 mmols) of (R)-(+)-5,11-dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]oxazepine in 20 ml of dichloromethane, and the mixture was stirred for 5 minutes. Then, the solvent was distilled off under reduced pressure. The resulting residue was recrystallized from a mixed solvent of dichloromethane and diethyl ether to give 2.9 g of (R)-(+)-5,11-dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]-dibenzo[b,e][1,4]oxazepine hydrochloride as a colorless prism crystal in a yield of 93%.

後処理

  1. distillationThen, the solvent was distilled off under reduced pressure
  2. customThe resulting residue was recrystallized from a mixed solvent of dichloromethane and diethyl ether

出典と根拠

ORDレコード
ord-5b99561e36e044bd8b1a5040104cdd7b
出典データセット
uspto-grants-2000_10
特許番号
US06127361

反応ノート

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