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Triethylamine → HCID 20552969、化合物

HRID 1446825
ノート
印刷プレビュー

反応式

HRID 1446825 の反応式
[NH2:1][C:2]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].C(OCl)(C)(C)C.[CH3:23][S:24][CH2:25][C:26]([NH:28][CH3:29])=[O:27].C(N(CC)CC)C>C(Cl)Cl>[NH2:1][C:2]1[C:3]([C:4](=[O:5])[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)=[CH:12][C:13]([Cl:16])=[CH:14][C:15]=1[CH:25]([S:24][CH3:23])[C:26]([NH:28][CH3:29])=[O:27]
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 8471TriethylamineHCID 128702-Amino-5-chlorobenzophenoneHCID 521297Tert-Butyl hypochloriteHCID 13553138HCID 13553138、化合物

生成物 1

HCID 20552969HCID 20552969、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 38.3 g (0.166 mole) of 2-amino-5-chlorobenzophenone in 1 liter of methylene chloride cooled to -70° C. under an atmosphere of nitrogen was added 18.05 g (0.167 mole) of t-butylhypochlorite. The solution was stirred for 15 min and then a solution of 20.3 g (0.171 mole) of 2-methylthio-N-methylacetamide in 100 ml of methylene chloride was added. The solution was stirred at -70° C. for 2 hrs and 25 ml of triethylamine was added. While stirring, the solution was allowed to warm to room temperature followed by extraction with water and drying of the organic layer with magnesium sulfate. The volume of the solution was reduced to about 400 ml, ether was added and the solution placed in a refrigerator at about 0° C. overnight. The solid which crystallized was dried under high vacuum for about 4 hr at 50° C. Weight of the product was 31.56 g (54.6%) which melted at 170°-171° C.

後処理

  1. stirringThe solution was stirred at -70° C. for 2 hrs
  2. stirringWhile stirring
  3. extractionfollowed by extraction with water
  4. dry with materialdrying of the organic layer with magnesium sulfate
  5. additionwas added
  6. waitthe solution placed in a refrigerator at about 0° C. overnight
  7. customThe solid which crystallized
  8. customwas dried under high vacuum for about 4 hr at 50° C

出典と根拠

ORDレコード
ord-f997dfa5412f40938ecb480c82e68ee2
出典データセット
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04313949

反応ノート

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