Hydrazine → 2-Hydrazinyl-5,6,7,8,9,10-hexahydrocycloocta[d]pyrimidine

HRID 2406132

反応式

HRID 2406132 の反応式
Cl[C:2]1[N:3]=[CH:4][C:5]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][C:6]=2[N:7]=1.[NH2:14][NH2:15]>N1C=CC=CC=1>[NH:14]([C:2]1[N:3]=[CH:4][C:5]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][C:6]=2[N:7]=1)[NH2:15]

参加物

4

反応物 2

HCID 9321HydrazineHCID 581995242-Chloro-5,6,7,8,9,10-hexahydrocycloocta[d]pyrimidine

生成物 1

HCID 552819292-Hydrazinyl-5,6,7,8,9,10-hexahydrocycloocta[d]pyrimidine

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

2-Chloro-5,6,7,8,9,10-hexahydrocycloocta[d]pyrimidine (1.5 g) was treated with anhydrous pyridine (15 mL) and anhydrous hydrazine (7 mL) at 120° C. for 3.75 h. The solvent was removed under vacuum. The residue was partitioned between chloroform and 1M aqueous potassium carbonate solution. The organic layer was dried over anhydrous sodium sulfate and concentrated under vacuum to give 2-hydrazinyl-5,6,7,8,9,10-hexahydrocycloocta[d]pyrimidine as a beige solid, 1.28 g; 1H NMR (CDCl3, 300 MHz) 8.00 (s, 1H), 6.63 (br s, 1H), 3.93 (br s, 2H), 2.76 (m, 2H), 2.60 (m, 2H), 1.74 (m, 2H), 1.63 (m, 2H), 1.40 (m, 4H) ppm; 13C NMR (CDCl3, 75 MHz) 170.57, 163.81, 157.22, 124.14, 34.31, 32.65, 30.24, 28.66, 26.32, 26.08; MS (ES) 193 (M+H).

後処理

  1. customThe solvent was removed under vacuum
  2. customThe residue was partitioned between chloroform and 1M aqueous potassium carbonate solution
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-1be71c0455ec464daaa0e0130f213446
出典データセット
uspto-grants-2014_08
特許番号
US08809347B2

関連ノート

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