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Water → 3-{(dibenzo[b,e]thiepin-11(6H)-yliden)-amino}-propyl tosylate

HRID 1287922
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HRID 1287922 반응식
[CH:1]1[C:11]2[C:10](=[N:12][CH2:13][CH2:14][CH2:15][OH:16])[C:9]3[CH:17]=[CH:18][CH:19]=[CH:20][C:8]=3[CH2:7][S:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.N1C=CC=CC=1.[C:27]1([CH3:37])[CH:32]=[CH:31][C:30]([S:33](Cl)(=[O:35])=[O:34])=[CH:29][CH:28]=1.O>C(Cl)Cl>[S:33]([C:30]1[CH:31]=[CH:32][C:27]([CH3:37])=[CH:28][CH:29]=1)([O:16][CH2:15][CH2:14][CH2:13][N:12]=[C:10]1[C:9]2[CH:17]=[CH:18][CH:19]=[CH:20][C:8]=2[CH2:7][S:6][C:5]2[CH:4]=[CH:3][CH:2]=[CH:1][C:11]1=2)(=[O:35])=[O:34]
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참가 물질

6

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HCID 962WaterHCID 1049PyridineHCID 73974-Toluenesulfonyl chlorideHCID 215070363-{(dibenzo[b,e]-thiepin-11(6H)-yliden)-amino}-1-propanol

생성물 1

HCID 215070443-{(dibenzo[b,e]thiepin-11(6H)-yliden)-amino}-propyl tosylate

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

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온도
0 °C

실험 절차

10.0 G. of 3-{ (dibenzo[b,e]thiepin-11(6H)-yliden)-amino}-1-propanol in 30 ml. of absolute pyridine are treated at 0° C. within 1 hour with 9.0 g. of p-toluenesulfonyl chloride. The solution is stirred at 0° C. for 1 hour and subsequently left to stand at 0° C. for 16 hours. The mixture is then diluted with methylene chloride and treated with water. The organic phase is washed with aqueous sodium bicarbonate solution, dried over sodium sulfate and evaporated under reduced pressure. There is obtained crude 3-{(dibenzo[b,e]thiepin-11(6H)-yliden)-amino}-propyl tosylate which is used in the reaction described in the first paragraph of this Example without further purification.

후처리

  1. waitsubsequently left
  2. waitto stand at 0° C. for 16 hours
  3. washThe organic phase is washed with aqueous sodium bicarbonate solution
  4. dry with materialdried over sodium sulfate
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-f3545eb9b7eb45fdab7dbf64e8545a83
출처 데이터셋
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03985895

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