Chloroacetonitrile → [(5-Chloro-1,3-benzothiazol-2-yl)sulfanyl]acetonitrile

HRID 325977노트

반응식

HRID 325977 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([SH:10])=[N:7][C:6]=2[CH:11]=1.Cl[CH2:13][C:14]#[N:15].C(N(CC)CC)C>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([S:10][CH2:13][C:14]#[N:15])=[N:7][C:6]=2[CH:11]=1

참가 물질

5

반응물 3

HCID 7856ChloroacetonitrileHCID 8471TriethylamineHCID 178527796HCID 178527796, 화합물

생성물 1

HCID 13312471[(5-Chloro-1,3-benzothiazol-2-yl)sulfanyl]acetonitrile

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

51.0 g (0.254 m), 5-chloro-2-mercaptobenzothiazole, 22.8 g (0.304 m) chloroacetonitrile and 30.7 g triethylamine are dissolved in 600 ml of toluene and the solution is heated to reflux for 3 hr, then allowed to cool to room temperature. The toluene solution is washed with water, dried over anhydrous magnesium sulfate and treated with Darco. After the solvent is removed, the residual solid is recrystallized from 300 ml. benzene. The recovered material is recrystallized from cyclohexane. A total yield of 52 g (86%) is obtained. The recrystallized sample has a melting point of 96°-7° C.

후처리

  1. temperaturethe solution is heated
  2. temperatureto reflux for 3 hr
  3. washThe toluene solution is washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. additiontreated with Darco
  6. customAfter the solvent is removed
  7. customthe residual solid is recrystallized from 300 ml
  8. customThe recovered material is recrystallized from cyclohexane
  9. customA total yield of 52 g (86%) is obtained

출처 및 근거

ORD 기록
ord-f11a01adcb744535b2e4d99644d3bd84
출처 데이터셋
uspto-grants-1984_04
특허 번호
US04443606

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