Hydrochloric Acid → (S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine hydrochloride

HRID 1460478ノート

反応式

HRID 1460478 の反応式
[ClH:1].[CH3:2][O:3][C:4]1[CH:32]=[CH:31][C:7]([CH2:8][CH2:9][N:10]2[CH2:14][CH2:13][CH2:12][C@H:11]2[CH2:15][N:16]2[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[CH2:20][S:19][C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]2=3)=[CH:6][CH:5]=1>CCOCC>[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[CH:6][C:7]([CH2:8][CH2:9][N:10]2[CH2:14][CH2:13][CH2:12][C@H:11]2[CH2:15][N:16]2[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[CH2:20][S:19][C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]2=3)=[CH:31][CH:32]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 9824029(S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine

生成物 1

HCID 67834802(S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine hydrochloride収率 43%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Excess saturated ethereal hydrogen chloride solution was added to a solution of (S)-5,11-dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine (see Examples 1 and 6) (1.30 g) in ether (20 ml) and the mixture was stirred at room temperature for 16 hours. The resulting precipitate was collected, washed several times with ether, dried and recrystallised from ethyl acetate to give the title compound as colourless crystals, (602 mg, 43%), m.p. 189°-190° C., [α]58925 -30.7° (c=0.57 in ethanol).

後処理

  1. customThe resulting precipitate was collected
  2. washwashed several times with ether
  3. customdried
  4. customrecrystallised from ethyl acetate

出典と根拠

ORDレコード
ord-a5f26e2f2374407f8ce6101c199d214e
出典データセット
uspto-grants-1991_12
特許番号
US05071844

反応ノート

読み込み中…