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Chloroform → 1,1'-[(Methanesulfinyl)methylene]bis(4-chlorobenzene)

HRID 2083099
ノート
印刷プレビュー

反応式

HRID 2083099 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.C(Cl)(Cl)Cl.[CH3:16][S:17][CH:18]([C:26]1[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][CH:27]=1)[C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1.C(=O)([O-])[O-].[K+].[K+]>O>[CH3:16][S:17]([CH:18]([C:19]1[CH:20]=[CH:21][C:22]([Cl:25])=[CH:23][CH:24]=1)[C:26]1[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][CH:27]=1)=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6212Chloroform2 回HCID 11430Potassium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 1770771,1'-[(Methylsulfanyl)methylene]bis(4-chlorobenzene)

生成物 1

HCID 1824941,1'-[(Methanesulfinyl)methylene]bis(4-chlorobenzene)収率 78.2%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

A solution of 10.7 grams (0.0525 mole) of m-chloroperbenzoic acid in 150 ml. of chloroform was slowly added to a cool solution (5°-7° C.) of 14.1 grams (0.050 mole) of bis(p-chlorophenyl)methyl methyl sulfide (prepared above) in 500 ml. of chloroform, and the resulting solution stirred for two hours at a temperature of 5° C., while a white precipitate formed. The mixture after warming to ambient temperature and holding at this temperature for a two hour period was then mixed with a solution having 20 grams of potassium carbonate in 200 ml. of water. The chloroform phase was then removed and washed with 100 ml. of water, and the chloroform distilled off by vacuum distillation leaving 14.7 grams of a crude product which was recrystallized twice from 2,2,4-trimethylpentane-benzene (2:1) mixture to yield 11.7 grams (78 percent) of the white colored solid of bis(p-chlorophenyl)methyl methyl sulfoxide with a melting point of 109.5°-110.5° C.

後処理

  1. customformed
  2. additionwas then mixed with a solution
  3. customThe chloroform phase was then removed
  4. washwashed with 100 ml
  5. distillationof water, and the chloroform distilled off by vacuum distillation
  6. customleaving 14.7 grams of a crude product which
  7. customwas recrystallized twice from 2,2,4-trimethylpentane-benzene (2:1) mixture

出典と根拠

ORDレコード
ord-b21f11e3493f4b73bbfb29ef5b7a9a9c
出典データセット
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04084005

反応ノート

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