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Formaldehyde → HCID 21427782、化合物

HRID 437268
ノート
印刷プレビュー

反応式

HRID 437268 の反応式
[CH2:1]=O.[CH3:3][C:4]([OH:13])([CH3:12])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH2:11]>O.C1C=CC=CC=1>[CH3:12][C:4]1([CH3:3])[C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[NH:11][CH2:1][O:13]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 2

HCID 712FormaldehydeHCID 2535272-(2-Aminophenyl)propan-2-ol

生成物 1

HCID 21427782HCID 21427782、化合物収率 58.5%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 962Water溶媒

実験手順

An 8.25-ml solution of 37% aqueous formaldehyde (0.099 mol) was added over 5 minutes to a cooled (0° C.) mixture of 10 g (0.066 mol) α,α-dimethyl-2-aminobenzyl alcohol in 50 ml water. The reaction mixture was then diluted with 50 ml benzene and vigorously stirred for 5 minutes. The aqueous layer was separated and extracted with benzene. The benzene layer of the reaction mixture and the benzene extracts were combined, dried over magnesium sulfate and evaporated. The resulting oil was distilled through a short column to give 6.3 g (b.p. 120° -125° C. at 0.1 mm of Hg) of 4,4-dimethyl-1,2-dihydro-4H-3,1-benzoxazine, as a colorless oil. Elemental analysis showed: %C, calc. 73.6, found 68.3: %H, calc. 8.0, found 7.6; %N, calc. 8.6, found 8.6.

後処理

  1. temperaturea cooled
  2. customThe aqueous layer was separated
  3. extractionextracted with benzene
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. distillationThe resulting oil was distilled through a short column

出典と根拠

ORDレコード
ord-f74a9330c1e14953bd442e710e4f60d7
出典データセット
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04030906

反応ノート

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