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Phosgene → HCID 15042235、化合物

HRID 1032093
ノート
印刷プレビュー

反応式

HRID 1032093 の反応式
[C:1]([Cl:4])(Cl)=[O:2].C(=O)([O-])[O-].[K+].[K+].C1(C(C2C=CC=CC=2)[N:18]2[CH2:21][CH:20]([O:22][C:23]3[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([Cl:30])[CH:24]=3)[CH2:19]2)C=CC=CC=1>C(Cl)Cl>[Cl:30][C:25]1[CH:24]=[C:23]([CH:28]=[CH:27][C:26]=1[Cl:29])[O:22][CH:20]1[CH2:19][N:18]([C:1]([Cl:4])=[O:2])[CH2:21]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6371PhosgeneHCID 11430Potassium CarbonateHCID 150422273-(3,4-Dichlorophenoxy)-1-(diphenylmethyl)azetidine

生成物 1

HCID 15042235HCID 15042235、化合物収率 70.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 14 g (0.144 mole) of phosgene in 200 ml of methylene chloride was treated with 19.9 g (0.144 mole) of anhydrous potassium carbonate and stirred for 1 hr, then 45.9 g (0.12 mole) of 1-diphenylmethyl-3-(3,4-dichlorophenoxy)azetidine in 100 ml of methylene chloride was added dropwise and stirring was continued for 72 hr. The reaction mixture was filtered to remove the inorganic salts and then concentrated in vacuo to a pale yellow oil (67 g). Trituration of the residue with cyclohexane yielded a crude pale yellow solid (23.6 g). The filtrate was treated with ligroin and upon standing, an additional 13.3 g of tacky material was obtained. After several recrystallizations from cyclohexane to remove traces of diphenylmethyl chloride a portion was obtained as fine white crystals, in 70.1% yield, m.p. 96°-99° C.

後処理

  1. stirringstirring
  2. waitwas continued for 72 hr
  3. filtrationThe reaction mixture was filtered
  4. customto remove the inorganic salts
  5. concentrationconcentrated in vacuo to a pale yellow oil (67 g)
  6. customTrituration of the residue with cyclohexane yielded a crude pale yellow solid (23.6 g)

出典と根拠

ORDレコード
ord-373cb395d73a4a42b1457bc3267b97de
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04956359

反応ノート

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