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

HRID 253298
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HRID 253298 반응식
[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
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참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-ef5c422be9b54f1f87964804f41eca4e
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07872014B2

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