Water → 7-(2-Chloro-6-fluorobenzylamino)[1,2,5]thiadiazolo[3,4-d]pyrimidine

HRID 1704778

反応式

HRID 1704778 の反応式
[NH2:1][C:2]1[C:3]2[C:4](=[N:8][S:9][N:10]=2)[N:5]=[CH:6][N:7]=1.[Cl:11][C:12]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[C:13]=1[CH2:14]N.O.CCCCCC>C(Cl)(Cl)Cl.CO>[Cl:11][C:12]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[C:13]=1[CH2:14][NH:1][C:2]1[C:3]2[C:4](=[N:8][S:9][N:10]=2)[N:5]=[CH:6][N:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 8058HexaneHCID 848332-Chloro-6-fluorobenzylamineHCID 95769(1,2,5)Thiadiazolo(3,4-d)pyrimidin-7-amine

生成物 1

HCID 204820257-(2-Chloro-6-fluorobenzylamino)[1,2,5]thiadiazolo[3,4-d]pyrimidine

試薬・触媒・溶媒 1

HCID 21584188Chloroform methanol溶媒

反応条件

温度
105 °C

実験手順

A flask was charged with 1.54 g. (0.01 mole) of 7-amino[1,2,5]thiadiazolo[3,4-d]pyrimidine prepared by the process set forth in Example 1 and 4.0 g. (0.025 mole) of 2-chloro-6-fluorobenzylamine prepared by the process set forth in Example 2. The suspension was stirred and heated at 105° C. for 18 hours. Ten ml. water and 20 ml. hexane were added in one portion and the resulting solid collected by filtration. The cake was washed with hexane and dried at 50° C. in vacuo to afford 2.86 g. (97%) of product. M.p. 224°-226° C.; tlc on silica gel in chloroform-methanol (8:1) showed a single fluorescent blue spot at Rf = 0.8; NMR (DMSO-d6) δ 4.92 (2H, s); 7.21 (broad s, 3H); 8.44 (s, 1H); 9.45 (s, 1H).

後処理

  1. additionA flask was charged with 1.54 g
  2. filtrationthe resulting solid collected by filtration
  3. washThe cake was washed with hexane
  4. customdried at 50° C. in vacuo
  5. customto afford 2.86 g

出典と根拠

ORDレコード
ord-56f1b9adde13466f9990db05be279ecb
出典データセット
uspto-grants-1978_11
特許番号
US04127721

関連ノート

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