Benzyl Chloride → N-benzyl-thiazolinethion

HRID 1581903

반응식

HRID 1581903 반응식
[CH2:1](Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([S:16][C:17]1[S:18][CH2:19][CH2:20][N:21]=1)C1C=CC=CC=1>CO>[CH2:1]([N:21]1[CH:20]=[CH:19][S:18][C:17]1=[S:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 7503Benzyl ChlorideHCID 2756772-Benzylthio-2-thiazoline

생성물 1

HCID 125489430N-benzyl-thiazolinethion수율 704.2%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
150 °C

실험 절차

12.7 g (0.1 mole) of benzylchloride were added to 209.2 g (1 mole) of 2-benzylthio-thiazoline and the mixture was heated to 150° C. for eight hours. The mixture was allowed to cool down to 70° C. and 500 ml of methanol were added. The reaction mixture was allowed to cool down to room temperature and stirred for an additional hour; N-benzyl-thiazoline-thion precipitated from the medium as a white crystalline product, was isolated by filtration and washed twice with 10 ml of methanol. The crude product was recrystallized from a minimum of acetonitrile. 146 g of N-benzyl-thiazolinethion were isolated and sulfonated as described below.

후처리

  1. temperatureto cool down to 70° C.
  2. temperatureto cool down to room temperature
  3. customN-benzyl-thiazoline-thion precipitated from the medium as a white crystalline product
  4. customwas isolated by filtration
  5. washwashed twice with 10 ml of methanol
  6. customThe crude product was recrystallized from a minimum of acetonitrile

출처 및 근거

ORD 기록
ord-789ad516cc7a459dbf3e7dacc4f95292
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06733947B2

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