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Triethylamine → 5-(Chloromethyl)-7-fluoro-2,3-dihydro-1,4-benzodioxine

HRID 253298
ノート
印刷プレビュー

反応式

HRID 253298 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:12]O)[C:5]2[O:10][CH2:9][CH2:8][O:7][C:6]=2[CH:11]=1.C(N(CC)CC)C.S(Cl)([Cl:23])=O>ClCCl>[Cl:23][CH2:12][C:4]1[C:5]2[O:10][CH2:9][CH2:8][O:7][C:6]=2[CH:11]=[C:2]([F:1])[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 66891450(7-Fluoro-2,3-dihydro-1,4-benzodioxine-5-yl)methanol

生成物 1

HCID 668901555-(Chloromethyl)-7-fluoro-2,3-dihydro-1,4-benzodioxine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of (7-fluoro-2,3-dihydro-1,4-benzodioxine-5-yl)methanol (436 mg, 2.36 mmol) and triethylamine (400 μL, 2.83 mmol) in dichloromethane (20 mL) was cooled to 0° C. and then slowly added thionyl chloride (260 μL, 3.55 mmol) and stirred for 45 min. The reaction mixture was partitioned with water (100 mL) and ethyl acetate (100 mL). The organic layer was washed with aqueous saturated sodium bicarbonate, brine, and then dried over anhydrous magnesium sulfate and concentrated to give crude 5-(chloromethyl)-7-fluoro-2,3-dihydro-1,4-benzodioxine as a colorless oil. The crude residue was taken up in N,N-dimethylformamide (10 mL) and was added potassium cyanide (460 mg, 7.08 mmol). The reaction mixture was heated to 60° C. and stirred for 5 h, at which time it was cooled to room temperature and partitioned with water (100 mL) and ethyl acetate (150 mL). The organic layer was washed with 10% citric acid (3×100 mL) and then aqueous saturated sodium bicarbonate (2×100 mL). The organic solution was further washed with brine, dried over anhydrous magnesium sulfate and concentrated to give 430 mg (94% over 2 steps) of (7-fluoro-2,3-dihydro-1,4-benzodioxin-5-yl)acetonitrile as an off-white powder. GCMS for C10H8FNO2: 193 (M+).

後処理

  1. customThe reaction mixture was partitioned with water (100 mL) and ethyl acetate (100 mL)
  2. washThe organic layer was washed with aqueous saturated sodium bicarbonate, brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-ef5c422be9b54f1f87964804f41eca4e
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07872014B2

反応ノート

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