Morpholine → HCID 71075618、化合物

HRID 2170658ノート

反応式

HRID 2170658 の反応式
[Cl:1][C:2]1[CH:25]=[CH:24][C:23]([O:26][C@@H:27]([CH3:32])[C:28]([O:30][CH3:31])=[O:29])=[CH:22][C:3]=1[CH2:4][N:5]1[C:13]2[C:8](=[CH:9][C:10]([C:14]([O:16]CC=C)=[O:15])=[CH:11][CH:12]=2)[C:7]([CH3:20])=[C:6]1[CH3:21].N1CCOCC1>C1COCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Cl:1][C:2]1[CH:25]=[CH:24][C:23]([O:26][C@@H:27]([CH3:32])[C:28]([O:30][CH3:31])=[O:29])=[CH:22][C:3]=1[CH2:4][N:5]1[C:13]2[C:8](=[CH:9][C:10]([C:14]([OH:16])=[O:15])=[CH:11][CH:12]=2)[C:7]([CH3:20])=[C:6]1[CH3:21]

参加物

5

反応物 2

HCID 8083MorpholineHCID 86674586HCID 86674586、化合物

生成物 1

HCID 71075618HCID 71075618、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of (S)-allyl 1-(2-chloro-5-((1-methoxy-1-oxopropan-2-yl)oxy)benzyl)-2,3-dimethyl-1H-indole-5-carboxylate (0.327 g, 0.72 mmol) and morpholine (0.63 mL, 7.2 mmol) in anhydrous THF (10 mL) was degassed, then Pd(PPh3)4 (0.083 g, 0.072 mmol) was added under argon protection. The reaction mixture was stirred at rt for 1 h. The solvent was removed and the resulting crude was dissolved in MeOH. The mixture was acidified with 2 N HCl to pH 3. The mixture was filtered and the solid was washed with water. The solid was dried for the next Step with no further purification. ESI-MS (m/z): 416 [M+1]+.

後処理

  1. customThe solvent was removed
  2. dissolutionthe resulting crude was dissolved in MeOH
  3. filtrationThe mixture was filtered
  4. washthe solid was washed with water
  5. customThe solid was dried for the next Step with no further purification

出典と根拠

ORDレコード
ord-27fda3059f2d4bcfa770adf2b84831c8
出典データセット
uspto-grants-2015_06
特許番号
US09051265B2

反応ノート

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