Hydrochloric Acid → NPSP795

HRID 2215279ノート

反応式

HRID 2215279 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])=[CH:5][C:4]=1[O:14][CH2:15][C@H:16]([OH:32])[CH2:17][NH:18][C:19]([CH3:31])([CH3:30])[CH2:20][CH:21]1[CH2:29][C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH2:22]1)#[N:2].[ClH:33]>C(#N)C.CCOCC>[ClH:33].[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])=[CH:5][C:4]=1[O:14][CH2:15][C@H:16]([OH:32])[CH2:17][NH:18][C:19]([CH3:30])([CH3:31])[CH2:20][CH:21]1[CH2:22][C:23]2[C:28](=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH2:29]1)#[N:2]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 9910902SB-423562

生成物 1

HCID 68607251NPSP795収率 94%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒

実験手順

The compound from Example 4 (80 mg, 0.18 mmol) was suspended in acetonitrile (8 mL) and treated with 1 N hydrogen chloride in ether dropwise with stirring until the solid dissolved. The mixture was quickly filtered and cooled in an ice bath. The white crystalline solid which formed was isolated by filtration, washed with ether, and dried in vacuo to afford the title compound (80 mg, 94%). Mp 180–181° C.; MS(ES) m/e 437.2 [M+H]+.

後処理

  1. dissolutiondissolved
  2. filtrationThe mixture was quickly filtered
  3. temperaturecooled in an ice bath
  4. customThe white crystalline solid which formed
  5. customwas isolated by filtration
  6. washwashed with ether
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-3564b0f2d4104ec38ab58cd32ac4b9a4
出典データセット
uspto-grants-2006_09
特許番号
US07109238B2

反応ノート

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