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Methanol → N-{[(2S)-4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}-N'-[(2-methyl-2H-tetraazol-5-yl)methyl]urea

HRID 1371450
ノート
印刷プレビュー

反応式

HRID 1371450 の反応式
Cl.[CH3:2][N:3]1[N:7]=[N:6][C:5]([CH2:8][NH2:9])=[N:4]1.Cl.[Cl:11][C:12]1[CH:13]=[C:14]([CH:36]=[CH:37][C:38]=1[Cl:39])[CH2:15][N:16]1[CH2:21][CH2:20][O:19][C@@H:18]([CH2:22][NH:23][C:24](=O)[O:25]C2C=CC([N+]([O-])=O)=CC=2)[CH2:17]1.C(N(CC)C(C)C)(C)C.CO>CN(C)C=O>[Cl:11][C:12]1[CH:13]=[C:14]([CH:36]=[CH:37][C:38]=1[Cl:39])[CH2:15][N:16]1[CH2:21][CH2:20][O:19][C@@H:18]([CH2:22][NH:23][C:24]([NH:9][CH2:8][C:5]2[N:6]=[N:7][N:3]([CH3:2])[N:4]=2)=[O:25])[CH2:17]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 81531DiisopropylethylamineHCID 13789253(2-methyl-2H-1,2,3,4-tetrazol-5-yl)methanamine hydrochlorideHCID 867603444-Nitrophenyl [(2S)-4-(3,4-dichlorobenzyl)morpholin-2-yl]methylcarbamate Hydrochloride

生成物 1

HCID 21070809N-{[(2S)-4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}-N'-[(2-methyl-2H-tetraazol-5-yl)methyl]urea収率 86.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Intermediate 30 (0.041 g) was added to a stirred solution of Intermediate 29 (0.110 g) in N,N-dimethylformamide (2 ml) at 22° C., and N,N-diisopropylethylamine (0.052 ml) was added. After stirring for 20 h, the mixture was applied in two equal portions to ion exchange cartridges (10 g Isolute SCX pre conditioned with methanol). Elution with methanol (3 column volumes) followed by 10% 0.880 ammonia in methanol (2 column volumes) and evaporation of the first basic fractions in vacuo gave the crude product. Purification by Biotage flash chromatography on silica gel (8 g cartridge), eluting with 100:8:1 dichloromethane/ethanol/0.880 ammonia, gave the title compound as a white solid, (0.0828 g).

後処理

  1. washElution with methanol (3 column volumes)
  2. customfollowed by 10% 0.880 ammonia in methanol (2 column volumes) and evaporation of the first basic fractions in vacuo
  3. customgave the crude product
  4. customPurification by Biotage flash chromatography on silica gel (8 g cartridge)
  5. washeluting with 100:8:1 dichloromethane/ethanol/0.880 ammonia

出典と根拠

ORDレコード
ord-8dc4361d18b449948acbb4e7a08b34a7
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07157457B2

反応ノート

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