Sodium Sulfate → HCID 11219349、化合物

HRID 2214966ノート

反応式

HRID 2214966 の反応式
[NH2:1][C@H:2]1[CH2:7][CH2:6][N:5](C(OC(C)(C)C)=O)[CH2:4][C@H:3]1[F:15].[O-]S([O-])(=O)=O.[Na+].[Na+].[N:23]1[C:31]2[C:26](=[N:27][CH:28]=[C:29]([CH:32]=O)[CH:30]=2)[S:25][N:24]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C(Cl)Cl.CCO>[F:15][C@@H:3]1[C@H:2]([NH:1][CH2:32][C:29]2[CH:30]=[C:31]3[N:23]=[N:24][S:25][C:26]3=[N:27][CH:28]=2)[CH2:7][CH2:6][NH:5][CH2:4]1

参加物

7

反応物 4

HCID 24436Sodium SulfateHCID 5049666Sodium triacetoxyborohydrideHCID 112644351,1-Dimethylethyl (3R,4S)-4-amino-3-fluoro-1-piperidinecarboxylateHCID 11355675[1,2,3]Thiadiazolo[5,4-b]pyridine-6-carbaldehyde

生成物 1

HCID 11219349HCID 11219349、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of cis-4-amino-1-tert-butoxycarbonyl-3-fluoropiperidine (1a) (1.00 mmole) in CH2Cl2 (5 mL) and EtOH (0.5 mL) is treated with anhydrous Na2SO4 (280 mg) and [1,2,3]thiadiazolo[5,4-b]pyridine-6-carboxaldehyde (1b) (1.10 mmole). The resulting solution is stirred at room temperature, then sodium triacetoxy borohydride (320 mg, 1.50 mmole) is added. The mixture is quenched by the addition of water (2 mL) and the volatiles removed in vacuo. Purification gives the desired compound.

後処理

  1. customThe mixture is quenched by the addition of water (2 mL)
  2. customthe volatiles removed in vacuo
  3. customPurification

出典と根拠

ORDレコード
ord-88034d44eb614e7f9ae9cd02985f40b3
出典データセット
uspto-grants-2006_09
特許番号
US07109213B2

反応ノート

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