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Hydrogen Bromide → HCID 63384188, 화합물

HRID 2400327
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HRID 2400327 반응식
[O:1]1[CH2:5][CH2:4][CH2:3][CH:2]1[C:6]1[S:10][C:9](N)=[N:8][N:7]=1.[BrH:12].N([O-])=O.[Na+]>O>[Br:12][C:9]1[S:10][C:6]([CH:2]2[CH2:3][CH2:4][CH2:5][O:1]2)=[N:7][N:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 40858925-(tetrahydrofuran-2-yl)-1,3,4-thiadiazol-2-amineHCID 23668193Sodium Nitrite

생성물 1

HCID 63384188HCID 63384188, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

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온도
0 °C

실험 절차

To 5-(Tetrahydro-furan-2-yl)-[1,3,4]thiadiazol-2-ylamine (0.5 g, 2.9 mmol) was added 48% HBr (7 ml) and H2O (7 ml). The reaction mixture was cooled to 0° C. using an icebath. Cu(I)Br (0.42 g, 2.9 mmol) was added, followed by a the dropwise addition of solution of NaNO2 (0.48 g, 10 mmol) in H2O (18 ml). The reaction mixture was stirred for a further 10 mins at 0° C. then allowed to warm up to room temperature over a 35 min period. A solution of saturated bicarbonated was added to the reaction mixture until the pH=6, then extracted with EtOAc, dried (MgSO4), filtered and the solvent removed in vacuo to afford the product (0.5 g, 2.1 mmol). MS: [M+H]+235, 237.

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후처리

  1. temperatureto warm up to room temperature over a 35 min period
  2. additionA solution of saturated bicarbonated was added to the reaction mixture until the pH=6
  3. extractionextracted with EtOAc
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-d0f0ef69494245f98bbd13a79987427b
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08796244B2

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