Triethylamine → 1,2-difluoro-3-isothiocyanatobenzene

HRID 1840369ノート

反応式

HRID 1840369 の反応式
[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]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10040ThiophosgeneHCID 782782,3-Difluoroaniline

生成物 1

HCID 27583301,2-difluoro-3-isothiocyanatobenzene収率 68.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-4bc40e1f9de54afe803912eae42780a0
出典データセット
uspto-grants-2004_01
特許番号
US06680317B2

反応ノート

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