Ammonia → HCID 178486132、化合物

HRID 1710368ノート

反応式

HRID 1710368 の反応式
[C:1]1([C:7]2[CH:8]=[C:9]3[N:15]=[C:14]([CH2:16][CH2:17][CH:18]4[N:24]=[C:23]([NH2:25])[CH2:22][CH2:21][CH2:20][CH2:19]4)[NH:13][C:10]3=[N:11][CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:26][N:27]([CH3:56])[S:28](C1C=CC(C2C=C3N=C(CCC4CCCCC(=S)N4)NC3=NC=2)=CC=1)(=[O:30])=[O:29].N>CO>[NH2:25][C:23]1[CH2:22][CH2:21][CH2:20][CH2:19][CH:18]([CH2:17][CH2:16][C:14]2[NH:13][C:10]3=[N:11][CH:12]=[C:7]([C:1]4[CH:2]=[CH:3][C:4]([S:28]([N:27]([CH3:56])[CH3:26])(=[O:30])=[O:29])=[CH:5][CH:6]=4)[CH:8]=[C:9]3[N:15]=2)[N:24]=1

参加物

5

反応物 3

HCID 222AmmoniaHCID 178486134N,N-dimethyl-4-{2-[2-(7-thioxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide2 回HCID 178508386HCID 178508386、化合物2 回

生成物 1

HCID 178486132HCID 178486132、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The title compound is synthesized as described for 7-[2-(6-phenyl-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-4,5,6,7-tetrahydro-3H-azepin-2-ylamine (compound 1) from 50 mg of N,N-dimethyl-4-{2-[2-(7-thioxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide (compound A5) and 2.53 ml of methanol containing ammonia (strength: 7.0 M) at 50° C. for 65 hours. Purification by flash chromatography on LiChroprep-NH2® (eluent: dichloromethane/0-10 vol. % methanol) and lyophilisation from dioxane/water (10:1 parts by volume) afford 32 mg of the title compound as an amorphous, colorless solid of m.p. 195° C. (decomp.). ESI-MS: 441.2 (MH+). TLC: Rf=0.44 (LiChroprep-NH2® HPTLC, methanol/water 10:1 parts by volume).

後処理

  1. customThe title compound is synthesized
  2. customPurification by flash chromatography on LiChroprep-NH2® (eluent: dichloromethane/0-10 vol. % methanol) and lyophilisation from dioxane/water (10:1 parts by volume)

出典と根拠

ORDレコード
ord-e8ba4f6bc32249179f5dd56742bf431a
出典データセット
uspto-grants-2010_09
特許番号
US07790710B2

反応ノート

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