Triethylamine → 1,2-difluoro-3-isothiocyanatobenzene

HRID 1840369노트

반응식

HRID 1840369 반응식
[F:1][C:2]1[C:8]([F:9])=[CH:7][CH:6]=[CH:5][C:3]=1[NH2:4].[C:10](Cl)(Cl)=[S:11].C(N(CC)CC)C>C1(C)C=CC=CC=1>[F:1][C:2]1[C:8]([F:9])=[CH:7][CH:6]=[CH:5][C:3]=1[N:4]=[C:10]=[S:11]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10040ThiophosgeneHCID 782782,3-Difluoroaniline

생성물 1

HCID 27583301,2-difluoro-3-isothiocyanatobenzene수율 68.7%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Into a solution of 2,3-difluoroaniline (1.0 g, 7.74 mmol) in 30 mL of toluene at room temperature, thiophosgene (0.91 mL, 11.6 mmol) and triethylamine (1.3 mL, 11.6 mmol) was added. The mixture was stirred at room temperature for 16 hours. The mixture was partitioned between ethyl acetate and water. The combined organic layer was then concentrated to give the desired product (910 mg, 68%). 1H NMR (CDCl3) δ 6.98 (m, 2H), 7.11 (m, 1H).

후처리

  1. customThe mixture was partitioned between ethyl acetate and water
  2. concentrationThe combined organic layer was then concentrated

출처 및 근거

ORD 기록
ord-4bc40e1f9de54afe803912eae42780a0
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06680317B2

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