Water → 3-(Phenyliminomethyl)dibenzo[b,f]thiepin-5,5-dioxide

HRID 485110ノート

反応式

HRID 485110 の反応式
[CH:1]1[C:11]2[CH:10]=[CH:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[S:6](=[O:17])(=[O:16])[C:5]=2[CH:4]=[C:3]([CH:18]=O)[CH:2]=1.[NH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.O>C1(C)C=CC=CC=1>[C:21]1([N:20]=[CH:18][C:3]2[CH:2]=[CH:1][C:11]3[CH:10]=[CH:9][C:8]4[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=4[S:6](=[O:17])(=[O:16])[C:5]=3[CH:4]=2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

参加物

5

反応物 3

HCID 962WaterHCID 6115AnilineHCID 13520245Dibenzo[b,f]thiepin-3-carboxaldehyde 5,5-dioxide

生成物 1

HCID 202715043-(Phenyliminomethyl)dibenzo[b,f]thiepin-5,5-dioxide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Heat a mixture of 675 mg (2.5 mmoles) of dibenzo[b,f]thiepin-3-carboxaldehyde-5,5-dioxide and 465 mg of aniline (5 mmoles) in 20 ml of toluene, under reflux, with azetropic removal of water for 21 hours. Cool the mixture and filter the insoluble product. Stir the solid in 10 ml of ether containing a few drops of THF for 10 minutes then filter to obtain the pure product, 704 mg, mp: 184°-185°.

後処理

  1. temperatureHeat
  2. temperatureCool the mixture
  3. filtrationfilter the insoluble product
  4. filtrationthen filter
  5. customto obtain the pure product, 704 mg, mp: 184°-185°

出典と根拠

ORDレコード
ord-54cc05676c3b4bd795500ef9ec0ae011
出典データセット
uspto-grants-1985_08
特許番号
US04535171

反応ノート

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