1,2-Dichloroethane → 3-(2-Thienylmethoxy)azetidine hydrochloride

HRID 2171986

反応式

HRID 2171986 の反応式
C1(C(C2C=CC=CC=2)[N:8]2[CH2:11][CH:10]([O:12][CH2:13][C:14]3[S:15][CH:16]=[CH:17][CH:18]=3)[CH2:9]2)C=CC=CC=1.[Cl:25]CCCl.ClC(OC(Cl)C)=O>CO>[ClH:25].[S:15]1[CH:16]=[CH:17][CH:18]=[C:14]1[CH2:13][O:12][CH:10]1[CH2:11][NH:8][CH2:9]1

参加物

5

反応物 3

HCID 111,2-DichloroethaneHCID 5213051-Chloroethyl chloroformateHCID 671546021-(Diphenylmethyl)-3-(2-thienylmethoxy)azetidine

生成物 1

HCID 671545443-(2-Thienylmethoxy)azetidine hydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

A 50 mL flask was charged with 1-(diphenylmethyl)-3-(2-thienylmethoxy)azetidine (204 mg, 0.61 mmol; which may be prepared as described in Step 2) and 1,2-dichloroethane (2.7 mL). 1-Chloroethyl chloroformate (86 μL, 0.79 mmol) was added and the reaction mixture was stirred at 70° C. for 1.5 h. After cooling to room temperature, methanol (2.7 mL) was added and the reaction mixture was stirred at 70° C. for 1.5 h. The reaction mixture was concentrated to dryness. The crude mixture was triturated in pentane to give a dark wax (140 mg, quantitative) which was used without further purification.

後処理

  1. temperatureAfter cooling to room temperature
  2. stirringthe reaction mixture was stirred at 70° C. for 1.5 h
  3. concentrationThe reaction mixture was concentrated to dryness
  4. customThe crude mixture was triturated in pentane
  5. customto give a dark wax (140 mg, quantitative) which
  6. customwas used without further purification

出典と根拠

ORDレコード
ord-1b19963750ac4979891e4080cf839359
出典データセット
uspto-grants-2015_06
特許番号
US09051321B2

関連ノート

読み込み中…