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3-Amino-1-propanol → 3-{(dibenzo[b,e]-thiepin-11(6H)-yliden)-amino}-1-propanol

HRID 1287921
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반응식

HRID 1287921 반응식
[CH:1]1[C:11]2[C:10](=O)[C:9]3[CH:13]=[CH:14][CH:15]=[CH:16][C:8]=3[CH2:7][S:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[NH2:17][CH2:18][CH2:19][CH2:20][OH:21]>O>[CH:1]1[C:11]2[C:10](=[N:17][CH2:18][CH2:19][CH2:20][OH:21])[C:9]3[CH:13]=[CH:14][CH:15]=[CH:16][C:8]=3[CH2:7][S:6][C:5]=2[CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 90863-Amino-1-propanolHCID 73741Dibenzo[b,e]thiepin-11(6H)-one

생성물 1

HCID 215070363-{(dibenzo[b,e]-thiepin-11(6H)-yliden)-amino}-1-propanol

시약·촉매·용매 1

HCID 962Water용매

실험 절차

30.0 G. of dibenzo[b,e]thiepin-11(6H)-one are heated to 180° C. with 300 ml. of 3-amino-1-propanol. The water formed and the excess amine are distilled off for 2 hours and the residue is then cooled, diluted with methylene chloride and washed several times with distilled water. The organic phase is dried over sodium sulfate and evaporated. After chromatographic purification over silica gel using toluene for the elution, there is obtained 3-{(dibenzo[b,e]-thiepin-11(6H)-yliden)-amino}-1-propanol.

후처리

  1. distillationthe excess amine are distilled off for 2 hours
  2. temperaturethe residue is then cooled
  3. additiondiluted with methylene chloride
  4. washwashed several times with distilled water
  5. dry with materialThe organic phase is dried over sodium sulfate
  6. customevaporated
  7. customAfter chromatographic purification over silica gel
  8. washfor the elution

출처 및 근거

ORD 기록
ord-2972d6e10af0459d97dea6bc94ec7d93
출처 데이터셋
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03985895

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