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

HRID 485110노트

반응식

HRID 485110 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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°.

후처리

  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°

출처 및 근거

ORD 기록
ord-54cc05676c3b4bd795500ef9ec0ae011
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04535171

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